HERBAL EXTRACT COMPOSITION AND A PROCESS THEREOF

Abstract
A composition is provided that includes extracts of green tea and rosemary extract optionally along with adjuvant and/or excipient. In addition, provided is a process for the preparation of said composition. Also provided is a composition including extract of green tea, rosemary extract and synthetic antioxidant optionally along with adjuvant and/or excipient.
Description
TECHNICAL FIELD

The present invention relates to a composition comprising extracts of green tea and rosemary extract optionally along with adjuvant and/or excipient. In addition, the present invention relates to a process for the preparation of said composition. The instant invention further relates to a composition comprising extract of green tea, rosemary extract and synthetic antioxidant optionally along with adjuvant and/or excipient.


BACKGROUND AND PRIOR ART OF THE INVENTION

Currently, food preservation systems often use chemicals and heat treatments to reduce the risk of bacterial food poisoning outbreaks and food spoilage, but chemicals can alter the taste of the product and, moreover, can compromise food safety.


In the past several years, a lot of work has been done in developing products that would serve as preservatives that could prevent the oxidation of fats, vegetable oils, carotenoids and their biologically active derivatives such as essential oils and other flavoring products so that the degradation of their quality is prevented in foodstuffs. Fats, oils and their products become rancid or unpleasant by odor or flavor due to the oxidative effects. The prior art shows various methods of inhibiting oxidation by addition of fat soluble antioxidants to the foodstuff. A number of chemical compounds are employed for avoiding or reducing these effects, so that, fats and oils or food containing fats and oils can be kept for longer periods of time. However, such agents have not been satisfactorily effective in many ways.


The chemical anti-oxidants that had been made use of in such cases include BHA (butylated hydroxyanisole), BHT (butylated hydroxyl toluene) and TBHQ (tertiary butyl hydroquinone) as well as other chemicals such as propyl gallate (PG). However, their volatility and tendency to decompose at higher temperature make them less suitable for deep fat or oil fried foods. Also, they were not found to be effective in protecting certain off-flavor development or the so called reversion flavor that occurs with the passage of time in oils like soybean oil.


It has been found that certain plant materials or extracts such as grape seed extracts, green tea extracts, sage, clove bud oil, clove leaf oil, Vitamin C, cinnamon leaf oil, oleoresin turmeric, tocopherol, tocotrienol, rosemary extracts and gallic acid etc., or salts thereof, were having anti-oxidant properties and their use as anti-oxidant preservatives have been widely discussed in past two decades. The use of natural anti-oxidants such as green tea as stabilizers for fats, oils, fatty food and ingredients of food is also discussed widely in U.S. Pat. No. 3,812,266 and U.S. Pat. No. 3,451,832. These patents describe the use of green tea and the importance of green tea catachin in the anti-oxidant activity of green tea. The work done in U.S. Pat. No. 4,840,966 and CA Patent No. 1057113A1 shows the health benefits of green tea and other such natural anti-oxidants.


Green tea is made from unfermented leaves and reportedly contains the highest concentration of powerful antioxidants called polyphenols, high antioxidant activity of green tea extracts, are used as a kind of innovative food additive to preserve pork, chicken meat, vegetable oil, fish oil and fish flesh, food emulsions and animal fat. Even though a number of antioxidants and various combinations thereof have been disclosed in the various inventions, there is still a need for additional antioxidant compositions in its right formulator form having improved characteristics.


With all the health benefits and the advantages of being all natural products, the use of such natural extracts needed further development of processes of extraction and the development of a right formulator form thereby making them effectively usable in such applications. The solubility factor is most important in such cases, where the formulated product had to be oil and fat soluble for them to be effective in their action as antioxidants.


In recent past several products are formulated for various application in fats and oil applications. Though the products developed from these natural products so far were found to be effective in their use as anti-oxidants, their use was not found satisfactory in terms of solubility factor with respect to time, sedimentation and extended shelf life in its use as preservatives in oils and fats and in processed foods such as deep fried foodstuffs. Thus, there was a need to develop a composition that can successfully overcome the difficulties stated above.


SUMMARY OF THE INVENTION

Accordingly the present disclosure relates to a composition comprising green tea extract and rosemary extract, optionally along with adjuvant or excipient or a combination thereof; a process of preparing the composition comprising green tea extract and rosemary extract, said process comprising acts of: a) granulating crude extract of green tea and mixing the granulated extract with the rosemary extract to obtain a mixture, b) optionally adding adjuvant or excipient or a combination thereof to the mixture, and c) passing the mixture of step a) or b) through homogenizer to obtain said composition comprising green tea extract and rosemary extract; a composition comprising the composition as mentioned above and tertiary butyl hydroquinone; an oil, fat or cosmetic preparation, comprising the composition as mentioned above; and a method of preparing the oil, fat or cosmetic preparation as mentioned above, wherein said method comprises act of mixing the composition as mentioned above with the oil, fat or cosmetic ingredients.





BRIEF DESCRIPTION OF THE ACCOMPANYING FIGURES


FIG. 1A illustrates Oxidative stability of palm oil at temperatures 100° C., 120° C. and 140° C. upon addition of instant composition, sample A, sample B, sample C, sample D, sample E and sample F, respectively.



FIG. 1B illustrates increase in the protection factor of palm oil at 100° C., upon addition of instant composition, sample A, sample B, sample C, sample D, sample E and sample F, respectively.



FIG. 1C illustrates increase in the protection factor of palm oil at 120° C., upon addition of instant composition, sample A, sample B, sample C, sample D, sample E and sample F, respectively.



FIG. 1D illustrates increase in the protection factor of palm oil at 140° C., upon addition of instant composition, sample A, sample B, sample C, sample D, sample E and sample F, respectively.



FIG. 2A illustrates Oxidative stability of sun flower oil at temperatures 80° C., 100° C. and 120° C. upon addition of instant composition, sample A, sample B, sample C, sample D, sample E and sample F, respectively.



FIG. 2B illustrates increase in the protection factor of sun flower oil at 80° C., upon addition of instant composition, sample A, sample B, sample C, sample D, sample E and sample F, respectively.



FIG. 2C illustrates increase in the protection factor of sun flower oil at 100° C., upon addition of instant composition, sample A, sample B, sample C, sample D, sample E and sample F, respectively.



FIG. 2D illustrates increase in the protection factor of sun flower oil at 120° C., upon addition of instant composition, sample A, sample B, sample C, sample D, sample E and sample F, respectively.



FIG. 3A illustrates Oxidative stability of almond oil at temperatures 100° C., 120° C. and 140° C. upon addition of instant composition, sample B, sample B1 and sample B2, respectively.



FIG. 3B illustrates increase in the protection factor of almond oil at 100° C., upon addition of instant composition, sample B, sample B1 and sample B2, respectively.



FIG. 3C illustrates increase in the protection factor of almond oil at 120° C., upon addition of instant composition, sample B, sample B1 and sample B2, respectively.



FIG. 3D illustrates increase in the protection factor of almond oil at 140° C., upon addition of instant composition, sample B, sample B1 and sample B2, respectively.



FIG. 4A illustrates Oxidative stability of apricot oil at temperatures 100° C., 120° C. and 140° C. upon addition of instant composition, sample B, sample B1 and sample B2, respectively.



FIG. 4B illustrates increase in the protection factor of apricot oil at 100° C., upon addition of instant composition, sample B, sample B1 and sample B2, respectively.



FIG. 4C illustrates increase in the protection factor of apricot oil at 120° C., upon addition of instant composition, sample B, sample B1 and sample B2, respectively.



FIG. 4D illustrates increase in the protection factor of apricot oil at 140° C., upon addition of instant composition, sample B, sample B1 and sample B2, respectively.



FIG. 5A illustrates Oxidative stability of fish oil at temperatures 60° C., 70° C. and 80° C. upon addition of instant composition, sample B2, sample C and sample D, respectively.



FIG. 5B illustrates increase in the protection factor of fish oil at 60° C., upon addition of instant composition, sample B2, sample C and sample D, respectively.



FIG. 5C illustrates increase in the protection factor of fish oil at 70° C., upon addition of instant composition, sample B2, sample C and sample D, respectively.



FIG. 6A illustrates peroxide value of palm oil at ambient temperature, upon addition of instant composition, sample A, sample B, sample C, sample D, sample E and sample F, respectively.



FIG. 6B illustrates peroxide value of palm oil at 50° C., upon addition of instant composition, sample A, sample B, sample C, sample D, sample E and sample F, respectively.



FIG. 6C illustrates para-anisidine value of palm oil at ambient temperature, upon addition of instant composition, sample A, sample B, sample C, sample D, sample E and sample F, respectively.



FIG. 6D illustrates para-anisidine value of palm oil at 50° C., upon addition of instant composition, sample A, sample B, sample C, sample D, sample E and sample F, respectively.



FIG. 6E illustrates totox value of palm oil at ambient temperature, upon addition of instant composition, sample A, sample B, sample C, sample D, sample E and sample F, respectively.



FIG. 6F illustrates totox value of palm oil at 50° C., upon addition of instant composition, sample A, sample B, sample C, sample D, sample E and sample F, respectively.



FIG. 7A illustrates peroxide value of sunflower oil at ambient temperature, upon addition of instant composition, sample A, sample B, sample C, sample D, sample E and sample F, respectively.



FIG. 7B illustrates peroxide value of sunflower oil at 50° C., upon addition of instant composition, sample A, sample B, sample C, sample D, sample E and sample F, respectively.



FIG. 7C illustrates para-anisidine value of sunflower oil at ambient temperature, upon addition of instant composition, sample A, sample B, sample C, sample D, sample E and sample F, respectively.



FIG. 7D illustrates para-anisidine value of sunflower oil at 50° C., upon addition of instant composition, sample A, sample B, sample C, sample D, sample E and sample F, respectively.



FIG. 7E illustrates totox value of sunflower oil at ambient temperature, upon addition of instant composition, sample A, sample B, sample C, sample D, sample E and sample F, respectively.



FIG. 7F illustrates totox value of sunflower oil at 50° C., upon addition of instant composition, sample A, sample B, sample C, sample D, sample E and sample F, respectively.



FIG. 8 illustrates peroxide value of fish oil at 10° C., upon addition of instant composition and alpha-tocopherol, respectively.



FIG. 9 illustrates total polar compound of palm oil, upon addition of instant composition, sample A, sample B, sample C, sample D, sample E and sample F, respectively.



FIG. 10 illustrates total polar compound of sunflower oil, upon addition of instant composition, sample A, sample B, sample C, sample D, sample E and sample F, respectively.



FIG. 11 illustrates relationship between particle size and antioxidant activity





DETAILED DESCRIPTION OF THE INVENTION

The present disclosure relates to a composition comprising green tea extract and rosemary extract, optionally along with adjuvant or excipient or a combination thereof.


In an embodiment the present disclosure relates to said green tea extract is at a concentration ranging from about 24% w/w to about 80% w/w.


In another embodiment the present disclosure relates to said rosemary extract is at a concentration ranging from about 45% w/w to about 85% w/w.


In yet another embodiment the present disclosure relates to said rosemary extract comprises rosemarinic acid at a concentration ranging from about 0.5% w/w to about 10% w/w, preferably at a range of about 0.5% w/w to about 3.5% w/w and carnosic acid at a concentration ranging from about 1.0% w/w to about 20% w/w, preferably at a range of about 1.5% w/w to about 12% w/w.


In still another embodiment the present disclosure relates to the adjuvant is selected from a group comprising vitamin C, gallic acid, vitamin E, rosmanol, ferulic acid, citric acid, mixed-tocopherol, lecithin, carotenoids and uric acid or any combination thereof.


In still another embodiment the present disclosure relates to the excipient is selected from a group comprising granulating agent, binding agent, lubricating agent, disintegrating agent, sweetening agent, glidant, anti-adherent, anti-static agent, surfactant, coating agent, colouring agent, flavouring agent, plasticizer, suspending agent, additive, emulsifying agent and spheronization agent or any combination thereof.


In still another embodiment the present disclosure relates to the emulsifying agent is polyglyceride fatty acid ester, preferably macrogoglycerol hydroxystearate; and wherein the additive is selected from a group comprising mono-di-glycerides, sorbitol, guar gum and xanthan gum or any combination thereof


In still another embodiment the present disclosure relates to said adjuvant at a concentration ranging from about 1.0 w/w to about 10% w/w, preferably ranging from about 1.5% w/w to about 8% w/w.


In still another embodiment the present disclosure relates to said excipient at a concentration ranging from about 0.5% to about 5% w/w, preferably ranging from about 1.0% w/w to about 2.5% w/w.


In still another embodiment the present disclosure relates to particle size of the composition ranging from about 5 μm to about 10 μm.


In still another embodiment the present disclosure relates to the composition optionally comprising polyphenols at a concentration ranging from about 30% to about 38%.


In still another embodiment the present disclosure relates to oil soluble composition having solubility ranging from about 95% to about 100% with settling less than about 0 about 5%.


The present disclosure further relates to a process of preparing the composition comprising green tea extract and rosemary extract, said process comprising acts of:

    • a. granulating crude extract of green tea and mixing the granulated extract with the rosemary extract to obtain a mixture;
    • b. optionally adding adjuvant or excipient or a combination thereof to the mixture; and
    • c. passing the mixture of step a) or b) through homogenizer to obtain said composition comprising green tea extract and rosemary extract


In an embodiment of the present disclosure, the crude extract of green tea having a particle size of about 50μ to about 200μ is granulated to obtain a extract of particle size ranging from about 10μ to about 20μ.


In another embodiment of the present disclosure, the composition obtained in step c) has a particle size ranging from about 5μ to about 10μ.


In yet another embodiment of the present disclosure, the crude extract of the green tea are granulated by techniques selected from a group comprising hammer mill, ball mill, plate mill, disc mill, colloid mill, micronisation method, high pressure homogenization and cryogenic grinding or a combination thereof, preferably cryogenic grinding.


In still another embodiment of the present disclosure, the mixing is carried out by an agitator at a speed of about 500 rpm to about 1000 rpm.


In still another embodiment of the present disclosure, the mixing is at a temperature ranging from about 40° C. to about 65° C., preferably at about 50° C. for time period ranging from about 2 hrs to about 24 hrs.


In still another embodiment of the present disclosure, the mixture is homogenized at a pressure ranging from about 500 bar to about 1000 bar.


The present disclosure further relates to a composition comprising the composition as mentioned above and tertiary butyl hydroquinone.


In an embodiment of the present disclosure, the composition as mentioned above is at a concentration ranging from about 50 ppm to about 100 ppm.


In another embodiment of the present disclosure, the tertiary butyl hydroquinone is at a concentration ranging from about 50 ppm to about 100 ppm.


The present disclosure further relates to an oil, fat or cosmetic preparation, comprising the composition of claim 1 or claim 20.


The present disclosure further relates to method of preparing the oil, fat or cosmetic preparation as claimed in claim 23, wherein said method comprises act of mixing the composition of claim 1 or claim 17 with the oil, fat or cosmetic ingredients.


The present invention provides an oil soluble composition comprising extract of green tea with rosemary extract, optionally along with adjuvants and excipients, wherein the composition is a natural antioxidant.


In an embodiment, the composition of the instant invention acts as a preservative in edible oil or cooking oil or food grade oil and oils which have cosmetic applications.


In an embodiment, the composition of the instant invention increases the oxidative induction time of the oil, thereby decreasing the rate of primary and secondary oxidation of the oil.


In an embodiment, the composition of the instant invention is added to oil at a concentration as low as about 50 ppm to as high as about 1000 ppm, unlike the conventionally known synthetic antioxidant, which have an upper limit of 200 ppm (under the regulatory guidelines) beyond which it is considered to be carcinogenic, whereas some antioxidant at higher dosage (above 500 ppm) acts as a pro-oxidant.


In an embodiment, the composition of the instant invention reduces the formation of polar compounds in the oil, thereby reducing degradation of oil. The composition of the instant invention also enhances the number of frying cycles at elevated temperatures and increases the shelf life of the oil.


In an embodiment, the oils for which the composition of instant invention acts as a preservative are avocado oil, mustard oil, palm oil, peanut oil, rice barn oil, safflower oil, sesame oil, sunflower oil, almond oil, canola oil, coconut oil, corn oil, cottonseed oil, mustard oil, grape seed oil, olive oil, pumpkin seed oil, tea seed oil, walnut oil, fish oil or any combination thereof.


In another embodiment, adjuvant of the instant composition is selected from a group comprising gallic acid, vitamin C, vitamin E, rosmanol, ferulic acid, citric acid, mixed-tocopherol, carotenoids and uric acid or any combination thereof. The excipient of the instant composition is selected from a group comprising granulating agent, binding agent, lubricating agent, disintegrating agent, sweetening agent, glidant, anti-adherent, anti-static agent, surfactant, coating agent, colouring agent, flavouring agent, plasticizer, suspending agent, emulsifying agent and spheronization agent or any combination thereof.


In an embodiment, the composition of the instant invention comprises about 24% w/w to about 80% w/w of green tea extract in powdered form and about 45% w/w to about 80% w/w of rosemary extract in oil form. The composition optionally comprises about 1% w/w to about 10% w/w, preferably from about 1.5% to about 8% w/w of one or more of adjuvants such as vitamin C, gallic acid, vitamin E, rosmanol, ferulic acid, citric acid, mixed-tocopherol, carotenoids, uric acid; optionally along with about 0.5% w/w to about 5% w/w, preferably from about 1.0% w/w to about 2.5% w/w excipients. The green tea extract in the composition of the instant invention is in the form of a powder made through cryogenic grinding with a particle size of about 10μ to about 200μ; and the rosemary is in the form of lipophilic extract containing rosemarinic acid at a concentration ranging from about 1.0% w/w to about 10% w/w, preferably from about 0.5% w/w to about 3.5% w/w and carnosic acid at a concentration ranging from about 1.0% w/w to about 20% w/w, preferably from about 1.5 w/w to about 12% w/w.


In an embodiment, the composition of the present invention comprises about 30% to about 38% of polyphenols, wherein the polyphenols content in the crude green tea extract is 90% and when this extract is cryo-grinded, mixed with rosemary extract optionally along with adjuvants and excipients, followed by high pressure homogenizing, the polyphenol content of PRESOL will be reduced to about 30% to about 38%, thereby enhancing the solubility of PRESOL.


In an embodiment, excipients, preferably, emulsifying agents enhances the solubility of the instant composition in oils, wherein the emulsifying agent is macrogoglycerol hydroxystearate. The instant composition comprising macrogogycerol hydroxystearate has a solubility ranging from about 95% to about 100% with settling less than about 5%.


In an embodiment, the instant composition comprises mono-di-glycerides as an additive.


In an embodiment, the composition of present invention is lipid soluble which prevents oxidative rancidity of oils and fats.


In an embodiment, the rosemary extract of the instant composition comprises rosemarinic acid or carnosic acid or a combination thereof.


The present invention further relates to a process of preparing a composition comprising extract of green tea with rosemary extract, optionally along with adjuvants and excipients, wherein said process comprises the following steps:

    • a) crude green tea extract with a particle size of 50μ to about 200μ is granulated to obtain a extract of particle size ranging from about 10μ to about 20μ;
    • b) an extract, sage or thyme of a Labiatae herb, preferably rosemary extract, is mixed with granulated green tea extract of particle size 10μ to about 20μ at a temperature ranging from about 40° C. to 65° C., preferably at about 50° C. for about 2 hrs to about 24 hrs, in a cylindrical vessel with an agitator rod with paddle that rotates at a speed of about 500 RPM to about 1200 RPM, to form a homogenous solution;
    • c) optionally adjuvants or excipients or a combination thereof is added to the solution, and mixed thoroughly to obtain a mixture;
    • d) the mixture of step d) is passed through high pressure homogenizer thrice at different pressures preferably in the range of about 500 bar to about 1000 bar, to obtain the final composition of the present invention.


In an embodiment, the green tea extract is granulated by any one or combination of the method selected from a group comprising hammer mill, ball mill, plate mill, disc mill, colloid mill, micronisation method, high pressure homogenization and cryogenic grinding.


In an embodiment, the crude green tea extract is granulated by cryogenic grinding to a particle size ranging from about 10μ to about 20μ


In an embodiment, the crude green tea extract before grinding is in the form of granular powder with a particle size ranging from about 50μ to about 200μ.


In an embodiment, the adjuvant is selected from a group comprising vitamin C, gallic acid, vitamin E, rosmanol, ferulic acid, citric acid, mixed-tocopherol, carotenoids and uric acid or any combination thereof.


In an embodiment, the excipient is selected from a group comprising granulating agent, binding agent, lubricating agent, disintegrating agent, sweetening agent, glidant, anti-adherent, anti-static agent, surfactant, coating agent, coloring agent, flavoring agent, plasticizer, suspending agent, emulsifying agent and spheronization agent or any combination thereof.


The present invention further relates to fortifying the composition comprising green tea extract and rosemary optionally along with adjuvant or excipients or a combination thereof with antioxidant selected from a group comprising butylated hydroxyanisole, butylated hydroxyl toluene, tertiary butyl hydroquinone, propyl gallate or any combination thereof, preferably butylated hydroxyl toluene.


In an embodiment, fortification of composition comprising green tea extract and rosemary extract optionally along with adjuvant or excipients or a combination thereof with antioxidant selected from a group comprising butylated hydroxyanisole, butylated hydroxyl toluene, tertiary butyl hydroquinone, propyl gallate or any combination thereof is carried out a concentration ranging from about 50 ppm to about 200 ppm, preferably in the range of about 50 ppm to about 100 ppm.


In an embodiment, present invention relates to an oil comprising green tea extract and rosemary extract, optionally along with adjuvant or excipients or a combination thereof, wherein the oil is edible oil or cooking oil or food grade oil, oil for cosmetic application, vegetable oil, plant oil or any combination thereof.


In another embodiment, present invention relates to an oil comprising green tea extract and rosemary extract, optionally along with adjuvant or excipients or a combination thereof, fortified with antioxidant selected from a group comprising butylated hydroxyanisole, butylated hydroxyl toluene, tertiary butyl hydroquinone, propyl gallate or any combination thereof, wherein the oil is edible oil or cooking oil or food grade oil, oil for cosmetic application, vegetable oil, plant oil or any combination thereof.


The further embodiment herein describes the scientific and technical terms used in connection with the instant invention and shall have meaning/definitions/equations/glossary that are commonly understood by those skilled in the art:


As used herein, ‘Oil Stability Index (OSI)’ is an American Oil Chemists Society (AOCS) approved method that determines the relative resistance of fat and oil samples to oxidation, which is defined by the following equation—







Oil





stability





index






(

O





S





I

)


=


Induction





time





of





treated





oil


Induction





time





of





control





oil






As used herein, ‘increase in protection factor’ is defined by the following equation—







Increase





in





protection





factor

=




O





S





I





of





treated





oil

-

O





S





I





of





control





oil



O





S





I





of





control





oil


×
100





As used herein, ‘PRESOL’ is the final composition of the instant invention, comprising extract of green tea with rosemary extract, optionally along with adjuvants and excipients.


As used herein, ‘crude green tea extract’ is a commercially available extract, obtained from green tea leaves (Camellia sinensis) having 90% polyphenol.


As used herein, ‘rosemary extract’ is commercially available extract which comprises rosemarinic acid at a concentration ranging from about 0.5% w/w to about 10% w/w and carnosic acid at a concentration ranging from about 1.0% w/w to about 20% w/w.


As used herein, ‘control’ is an oil without any antioxidant.


As used herein, ‘Sample A’ is oil with TBHQ (98% activity)


As used herein, ‘Sample B’ is oil with BHA (98% activity)


As used herein, ‘Sample C’ is oil with pulverized green tea (95% polyphenols)


As used herein, ‘Sample D’ is oil with rosemary extract (8% Carnosic acid)


As used herein, ‘Sample E’ is oil with cryogrinded green tea (95% Polyphenols) As used herein, ‘Sample B1’ is oil with BHA (98% activity)


As used herein, ‘Sample B2’ is oil with alpha tocopherol (96% activity)


The present invention is further illustrated by the following examples. However, the following examples are provided for illustrative purposes only and are not intended to limit the scope of the invention.


EXAMPLES
Example 1
Process of Preparing PRESOL





    • a. In order to prepare 1000 g of PRESOL, 500 g of crude green tea extract with a particle size of about 50μ to about 200μ is cryo-grinded for two cryo cycles for about 10 mins each with an intermediate cooling for about 1 minute. 470 g of green tea extract is recovered from the cryo-grinder, with a particle size of about 10μ to about 20μ. To 300 g of the cryo-grinded green tea extract, about 500 g of rosemary extract comprising 11.67% carnosic acid is added and mixed slowly in a cylindrical vessel with an agitator rod with paddle that rotates at a speed of about 500 RPM to about 1200 RPM at a temperature of about 40° C. to about 65° C. for about 2 hrs to about 24 hrs to obtain a mixture. To the mixture, 50 g of vitamin C, 50 g of Tocopherol, 50 g of lecithin, 90 g of mono-di-glycerides and 10 g of Macrogoglycerol hydroxystearate is added. This obtained mixture is mixed thoroughly and passed through a high pressure homogenizer at three different pressures in the range of about 500 bar to about 1000 bar to obtain PRESOL with a yield of about 93.5%.

    • b. In order to prepare 500 g of PRESOL, 250 g of crude green tea extract with a particle size of about 50μ to about 200μ is cryo-grinded for two cryo cycles for about 10 mins each with an intermediate cooling for about 1 minute. 235 g of green tea extract is recovered from the cryo-grinder, with a particle size of about 10μ to about 20μ. To 150 g of the cryo-grinded green tea extract, about 250 g of rosemary extract comprising 11.67% carnosic acid is added and mixed slowly in a cylindrical vessel with an agitator rod with paddle that rotates at a speed of about 500 RPM to about 1200 RPM at a temperature of about 40° C. to about 65° C. for about 2 hrs to about 24 hrs to obtain a mixture. This mixture is mixed thoroughly and passed through a high pressure homogenizer at three different pressures in the range of about 500 bar to about 1000 bar to obtain PRESOL with a yield of about 93.5%.





Example 2
Oil Stability Index

The oil stability index is determined using the Metrohm's Rancimat (Metrohm 743 Rancimat).


A. Oil Stability Index of Palm Oil


4.0 g of palm oil is weighed into the reaction vessel. The reaction vessel filled with oil is placed in a heating block. The temperature of the block is maintained at 100° C., 120° C. and 140° C., respectively. The oil is heated at the said temperatures, followed by passing air at a flow rate of 20 L/h. Flowing of air through the oil produces peroxides during primary oxidation and organic acids having low molecular weight, aldehydes and ketones with typical rancid odor during the secondary oxidation phase. These compounds are conveyed by the air flow into measurement vessel containing distilled water where conductivity is being checked continuously by sensor. Variation in conductivity of water shows the presence of organic acids, thus analyzing the induction time of the oil.


The above experiment is repeated by adding 200 ppm of TBHQ (sample-A), 200 ppm of BHA (sample-B), 200 ppm of pulverized green tea extract with 90% polyphenol (sample-C), 200 ppm of rosemary (sample-D), 200 ppm of green tea extract after cryogenic grinding (sample-E), 200 ppm of crude green tea extract (sample-F) and PRESOL at 200 ppm, 500 ppm and 1000 ppm, respectively to palm oil.


From the above experiment, oxidative stability index of untreated oil (control) and treated oil is calculated and the below table illustrates the induction time and the obtained oxidative stability.









TABLE 1







Oxidative Stability of Palm oil











Oxidative Stability



Induction Time (h)
Index (OSI)













Treatment
100° C.
120° C.
140° C.
100° C.
120° C.
140° C.
















Control PO
41.7
9.64
2.45
1.00
1.00
1.00


Sample A
95.76
20.93
5.26
2.30
2.17
2.15


Sample B
43.33
9.88
2.51
1.04
1.02
1.02


Sample C
74.22
17.95
4.48
1.78
1.86
1.83


Sample D
54.85
13.32
3.14
1.32
1.38
1.28


Sample E
82.46
20.02
4.95
1.98
2.08
2.02


Sample F
58.23
14.17
3.45
1.40
1.47
1.41


PRESOL
63.59
15.57
3.86
1.52
1.62
1.58


PRESOL
97.4
23.74
5.62
2.34
2.46
2.29


PRESOL
135.8
33.64
8.14
3.26
3.49
3.32









Based on the obtained oxidative stability index (illustrated in FIG. 1A), protection factor for the samples are assessed at temperatures 100° C., 120° C. and 140° C. to analyze the increase in the protection factor, which in turn illustrates the enhancement in oxidative stability obtained by treating the oil with PRESOL, TBHQ, BHA, pulverized green tea extract, rosemary extract, green tea extract after cryogenic grinding and crude green tea extract. FIGS. 1B, 1C and 1D illustrate the increase in the protection factor by treating the oil with PRESOL. Further table 1 illustrates substantial enhancement of oxidative stability of palm oil with PRESOL.


B. Oil Stability Index of Sunflower Oil


4.0 g of sunflower oil is weighed into the reaction vessel. The reaction vessel filled with oil is placed in a heating block. The temperature of the block is maintained at 80° C., 100° C. and 120° C., respectively. The oil is heated at the said temperatures, followed by passing air at a flow rate of 20 L/h. Flowing of air through the oil produces peroxides during primary oxidation and organic acids having low molecular weight, aldehydes and ketones with typical rancid odor during the secondary oxidation phase. These compounds are conveyed by the air flow into measurement vessel containing distilled water where conductivity is being checked continuously by sensor. Variation in conductivity of water shows the presence of organic acids, thus analyzing the induction time of the oil.


The above experiment is repeated by adding 200 ppm of TBHQ (sample-A), 200 ppm of BHA (sample-B), 200 ppm of pulverized green tea extract with 90% polyphenol (sample-C), 200 ppm of rosemary extract (sample-D), 200 ppm of green tea extract after cryogenic grinding (sample-E), 200 ppm of crude green tea extract (sample-F) and PRESOL at 200 ppm, 500 ppm and 1000 ppm, respectively to sunflower oil. From the above experiment, oxidative stability index of untreated oil (control) and treated oil is calculated and the below table illustrates the induction time and the obtained oxidative stability.









TABLE 2







Oxidative Stability index of sunflower oil











Oxidative Stability



Induction Time (h)
Index (OSI)













Treatment
80° C.
100° C.
120° C.
80° C.
100° C.
120° C.
















Control SFO
36.48
9.32
2.35
1.00
1.00
1.00


Sample A
109.76
26.82
6.13
3.01
2.88
2.61


Sample B
50.39
13.33
2.64
1.38
1.43
1.12


Sample C
98.52
24.03
5.48
2.70
2.58
2.33


Sample D
52.19
12.94
2.85
1.43
1.39
1.21


Sample E
102.85
25.28
6.05
2.82
2.71
2.57


Sample F
78.42
19.08
4.55
2.15
2.05
1.94


PRESOL
76.52
18.38
4.29
2.10
1.97
1.83


PRESOL
93.18
22.76
5.47
2.55
2.44
2.33


PRESOL
139.72
34.41
8.38
3.83
3.69
3.57









Based on the obtained oxidative stability index (illustrated in FIG. 2A), protection factor for the samples are assessed at temperatures 80° C., 100° C. and 120° C. to analyze the increase in the protection factor, which in turn illustrates the enhancement in oxidative stability obtained by treating the oil with PRESOL, TBHQ, BHA, pulverized green tea extract, rosemary extract, green tea extract after cryogenic grinding and crude green tea extract. FIGS. 2B, 2C and 2D illustrate the increase in the protection factor by treating sunflower oil with PRESOL. Further table 2 illustrates substantial enhancement of oxidative stability of palm oil with PRESOL.


Lower temperature is chosen to study the oxidative stability of sunflower oil, because sunflower is less stable at higher temperatures when compared to palm oil.


C. Oil Stability Index of Almond Oil


4.0 g of almond oil is weighed into the reaction vessel. The reaction vessel filled with oil is placed in a heating block. The temperature of the block is maintained at 100° C., 120° C. and 140° C., respectively. The oil is heated at the said temperatures, followed by passing air at a flow rate of 20 L/h. Flowing of air through the oil produces peroxides during primary oxidation and organic acids having low molecular weight, aldehydes and ketones with typical rancid odor during the secondary oxidation phase. These compounds are conveyed by the air flow into measurement vessel containing distilled water where conductivity is being checked continuously by sensor. Variation in conductivity of water shows the presence of organic acids, thus analyzing the induction time of the oil.


The above experiment is repeated by adding 200 ppm of BHA (sample-B), 200 ppm of BHT (sample-B1), 500 ppm of alpha tocopherol (sample-B2) and PRESOL at 200 ppm, 500 ppm and 1000 ppm, respectively to almond oil. From the above experiment, oxidative stability index of untreated oil (control) and treated oil is calculated and the below table illustrates the induction time and the obtained oxidative stability.









TABLE 3







Oxidative Stability index of almond oil











Oxidative Stability



Induction Time
Index (OSI)













Treatment
100° C.
120° C.
140° C.
100° C.
120° C.
140° C.
















Control
22.09
5.06
1.37
1.00
1.00
1.00


Almond Oil


Sample B
25.14
6.11
1.52
1.14
1.21
1.11


Sample B1
24.98
5.89
1.48
1.13
1.16
1.08


Sample B2
24.51
5.73
1.43
1.11
1.13
1.04


PRESOL
30.16
7.48
1.77
1.37
1.48
1.29


PRESOL
45.37
11.00
2.65
2.05
2.17
1.93


PRESOL
62.13
15.05
3.62
2.81
2.97
2.64









Based on the obtained oxidative stability index (illustrated in FIG. 3A), protection factor for the samples are assessed at temperatures 100° C., 120° C. and 140° C. to analyze the increase in the protection factor, which in turn illustrates the enhancement in oxidative stability obtained by treating the oil with PRESOL, BHA, BHT and alpha tocopherol. FIGS. 3B, 3C and 3D illustrate the increase in the protection factor by treating almond oil with PRESOL. Further table 3 illustrates substantial enhancement of oxidative stability of almond oil with PRESOL.


D. Oil Stability Index of Apricot Oil


4.0 g of apricot oil is weighed into the reaction vessel. The reaction vessel filled with oil is placed in a heating block. The temperature of the block is maintained at 100° C., 120° C. and 140° C., respectively. The oil is heated at the said temperatures, followed by passing air at a flow rate of 20 L/h. Flowing of air through the oil produces peroxides during primary oxidation and organic acids having low molecular weight, aldehydes and ketones with typical rancid odor during the secondary oxidation phase. These compounds are conveyed by the air flow into measurement vessel containing distilled water where conductivity is being checked continuously by sensor. Variation in conductivity of water shows the presence of organic acids, thus analyzing the induction time of the oil.


The above experiment is repeated by adding 200 ppm of BHA (sample-B), 200 ppm of BHT (sample-B1), 500 ppm of alpha tocopherol (sample-B2) and PRESOL at 200 ppm, 500 ppm and 1000 ppm, respectively to apricot oil. From the above experiment, oxidative stability index of untreated oil (control) and treated oil is calculated and the below table illustrates the induction time and the obtained oxidative stability.









TABLE 4







Oxidative Stability index of apricot oil










Induction Time
Oxidative Stability



at 200 ppm
Index (OSI)













Treatment
100° C.
120° C.
140° C.
100° C.
120° C.
140° C.
















Control
26.88
5.87
1.48
1.00
1.00
1.00


Apricot Oil


Sample B
29.16
6.66
1.57
1.08
1.13
1.06


Sample B1
26.96
5.93
1.49
1.00
1.01
1.01


Sample B2
22.06
5.06
1.32
0.82
0.86
0.89


PRESOL
33.68
8.43
1.88
1.25
1.44
1.27


PRESOL
45.22
10.15
2.46
1.68
1.73
1.66


PRESOL
56.19
13.88
3.29
2.09
2.36
2.22









Based on the obtained oxidative stability index (illustrated in FIG. 4A), protection factor for the samples are assessed at temperatures 100° C., 120° C. and 140° C. to analyze the increase in the protection factor, which in turn illustrates the enhancement in oxidative stability obtained by treating the oil with PRESOL, BHA, BHT and alpha tocopherol. FIGS. 4B, 4C and 4D illustrate the increase in the protection factor by treating apricot oil with PRESOL. Further table 4 illustrates substantial enhancement of oxidative stability of apricot oil with PRESOL.


E. Oil Stability Index of Fish Oil


4.0 g of fish oil is weighed into the reaction vessel. The reaction vessel filled with oil is placed in a heating block. The temperature of the block is maintained at 60° C., 70° C. and 80° C., respectively. The oil is heated at the said temperatures, followed by passing air at a flow rate of 20 L/h. Flowing of air through the oil produces peroxides during primary oxidation and organic acids with low molecular weight, aldehydes and ketones with typical rancid odor during the secondary oxidation phase. These compounds are conveyed by the air flow into measurement vessel containing distilled water where conductivity is being checked continuously by sensor. Variation in conductivity of water shows the presence of organic acids, thus analyzing the induction time of the oil.


The above experiment is repeated by adding, 200 ppm of alpha tocopherol (sample-B2), 200 ppm of pulverized green tea extract with 90% polyphenol (sample-C), 200 ppm of rosemary extract (sample-D) and PRESOL at 200 ppm, 500 ppm and 1000 ppm, respectively to fish oil. From the above experiment, oxidative stability index of untreated oil (control) and treated oil is calculated and the below table illustrates the induction time and the obtained oxidative stability.









TABLE 5







Oxidative Stability index of Fish oil











Oxidative Stability



Induction Time
Index (OSI)













Treatment
80° C.
70° C.
60° C.
80° C.
70° C.
60° C.
















Control Fish oil
2.46
4.98
9.86
1.00
1.00
1.00


Sample B2
6.78
13.74
27.68
2.76
2.76
2.81


Sample D
1.97
4.05
8.36
0.80
0.81
0.85


Sample C
2.28
4.74
9.75
0.93
0.95
0.99


PRESOL at
3.07
6.32
13.04
1.25
1.27
1.32


200 ppm


PRESOL at
4.78
9.68
19.85
1.94
1.94
2.01


500 ppm


PRESOL at
8.02
16.14
33.07
3.26
3.24
3.35


1000 ppm









Based on the obtained oxidative stability index (illustrated in FIG. 5A), protection factor for the samples are assessed at temperatures 60° C., 70° C. and 80° C. to analyze the increase in the protection factor, which in turn illustrates the enhancement in oxidative stability obtained by treating the oil with PRESOL, alpha tocopherol, pulverized green tea extract with 90% polyphenol and rosemary extract. FIGS. 5B, 5C and 5D illustrate the increase in the protection factor by treating fish oil with PRESOL. Further table 5 illustrates substantial enhancement of oxidative stability of fish oil with PRESOL.


Example 3

An extension of the Example 1 is provided by a new function known as temperature extrapolation. This is an aid for estimating the shelf life of oils and fats. The extrapolation makes use of the relationship between the measured induction time and the temperature given by van't Hoff's law. Several measurements are made at different temperatures and then extrapolated to the storage temperature. The values so obtained allow estimation of the storage stability of the oil or fat containing PRESOL.


The shelf life is calculated using Rancimat shelf life calculator. The shelf life of oil is studied by carrying out chemical analysis, which include studying peroxide value (represents extent of primary oxidation), Para-anisidine value (represents extent of secondary oxidation) and totox value (reflects total oxidation of oil). These parameters are determined for 1 kg of untreated oil and treated oil at every 15 days interval for samples stored at ambient temperature and at every 7 days interval for samples stored at 50° C. The treated oil being, the oil upon addition of 200 ppm of TBHQ (sample-A), 200 ppm of BHA (sample-B), 200 ppm and 500 ppm of pulverized green tea extract with 90% polyphenol (sample-C), 200 ppm and 500 ppm of rosemary extract (sample-D), 200 ppm and 500 ppm of green tea extract after cryogenic grinding (sample-E), 200 ppm and 500 ppm of crude green tea extract (sample-F) and PRESOL at 200 ppm and 500 ppm. The untreated oil is the control sample without any antioxidant.


The threshold limit for per oxide value under which oil can be used for safe consumption is 10 meq of O2/Kg oil. Similarly, the threshold limit of para-anisidine value and Totox value is 10 and 30, respectively.


A. Determination of Shelf Life of Palm Oil









TABLE 6







Estimation of Shelf life of Palm oil










Treatment
Shelf Life (days) at 30° C.







Control
242.9



Sample A
617.0



Sample B
260.9



Sample C
420.8



Sample D
337.8



Sample E
475.1



Sample F
337.4



PRESOL
356.7



PRESOL
606.0



PRESOL
790.8










Table 6 illustrates that PRESOL suitably enhances the shelf life of palm oil.









TABLE 7







Peroxide value of palm oil at ambient temperature






















sample
Sample
Sample













A
B
C
Sample D
Sample E
Sample
PRESOL
Sample C
Sample D
Sample E
Sample F
PRESOL



Control
at 200
at 200
at 200
at 200
at 200
F at 200
at 200
at 500
at 500
at 500
at 500
at 500


Day
PO
ppm
ppm
ppm
ppm
ppm
ppm
ppm
ppm
ppm
ppm
ppm
ppm























0
0.465
0.465
0.465
0.465
0.465
0.465
0.465
0.465
0.465
0.465
0.465
0.465
0.465


15
0.948
0.762
0.868
0.904
0.903
0.92
0.941
0.817
0.842
0.61
0.87
0.903
0.77


30
2.053
1.417
1.691
0.955
1.023
0.94
0.968
0.871
0.907
1.018
0.969
0.974
0.85


45
2.838
1.558
2.684
1.015
1.478
0.973
1.104
0.995
1.037
1.488
0.995
1.098
0.949


60
3.523
1.771
4.034
1.956
1.834
1.912
2.074
1.864
1.946
1.893
2.016
2.101
1.753


75
3.879
1.855
4.748
2.626
2.973
2.62
2.793
2.008
2.425
2.714
2.725
2.86
1.823


90
4.51
1.814
5.034
2.635
3.336
2.621
2.673
2.205
2.622
3.154
2.664
2.787
1.856


105
5.893
1.88
5.316
2.68
3.463
2.671
2.67
2.305
2.646
3.347
2.754
2.68
1.934


120
7.163
1.91
6.307
2.735
3.826
2.715
2.763
2.5
2.766
3.613
2.866
2.957
2.076


135
8.15
1.951
7.887
2.764
4.096
2.75
2.807
2.701
2.702
3.776
2.803
2.811
2.143


150
8.807
2.222
8.617
2.798
4.471
2.788
2.901
2.802
2.812
4.051
2.825
2.866
2.224


165
10.481
2.31
11.307
2.886
4.804
2.879
3.092
2.832
2.917
4.717
2.942
3.094
2.309


180
13.712
2.403
12.75
3.229
4.967
3.149
3.505
3.032
3.127
4.787
3.218
3.457
2.501









Table 7 and FIG. 6A illustrates that PRESOL at 500 ppm is showing equivalent efficacy in preventing oxidative rancidity as compared to 200 ppm of sample A in palm oil at ambient temperatures. From tables 6 and 7, it is further evident that 500 ppm PRESOL is having efficacy equivalent to 200 ppm Sample A. On the other hand control and sample B are crossing threshold limit after 165 days.









TABLE 8







Peroxide value of palm oil at 50° C.






















sample
Sample
Sample













A
B
C
Sample D
Sample
Sample
PRESOL
Sample
Sample
Sample
Sample
PRESOL



Control
at 200
at 200
at 200
at
E at
F at
at 200
C at
D at
E at
F at 500
at 500


Day
PO
ppm
ppm
ppm
200 ppm
200 ppm
200 ppm
ppm
500 ppm
500 ppm
500 ppm
ppm
ppm























0
0.482
0.482
0.482
0.482
0.482
0.482
0.482
0.482
0.482
0.482
0.482
0.482
0.482


7
6.11
1.309
4.735
1.355
2.52
0.743
2.266
1.272
1.358
2.516
0.752
2.249
1.216


15
10.076
1.836
9.973
2.558
3.711
1.63
3.019
2.053
2.606
2.483
1.585
2.867
1.705


22
13.901
1.887
13.062
3.155
4.26
2.077
4.044
2.657
3.046
4.084
2
3.657
1.906


30
17.929
2.005
16.45
4.166
5.485
2.601
4.677
2.693
4.344
3.508
2.584
4.686
2.123


37
36.394
3.074
35.595
5.016
10.528
2.892
5.606
3.016
5.115
6.806
2.806
5.563
2.966


45
61.424
3.686
60.884
6.11
15.1
3.431
6.693
3.903
5.944
9.745
3.387
6.635
3.503


52
50.607
4.102
51.15
6.562
12.969
4.201
7.062
4.485
6.589
9.892
4.027
6.868
4.106


60
30.568
4.491
42.269
7.485
15.711
7.583
8.848
4.891
7.053
11.688
7.482
8.656
4.505


67
24.515
4.75
34.974
8.064
18.284
7.884
10.141
5.159
8.238
13.004
7.49
9.022
4.639


75
15.389
4.893
25.576
9.503
22.92
8.277
11.689
5.714
8.726
14.769
7.945
10.885
4.911


82
10.65
5.209
11.31
14.953
25.251
11.106
17.905
5.955
14.342
24.801
10.292
17.121
5.484


90
12.991
5.395
15.231
19.053
27.907
13.438
22.441
6.502
18.637
26.983
13.188
21.396
5.813









Table 8 and FIG. 6B illustrates that after 90 days of storage at 50° C., PRESOL at 200 ppm and 500 ppm does not cross threshold limit and are acting similar to sample A.









TABLE 9







Para-anisidine value of palm oil at ambient temperature






















sample
Sample
Sample
Sample
Sample
Sample
PRESOL
Sample
Sample
Sample
Sample
PRESOL




A at
B at
C at
D at
E at
F at
at
C at
D at
E at
F at
at



Control
200
200
200
200
200
200
200
500
500
500
500
500


Day
PO
ppm
ppm
ppm
ppm
ppm
ppm
ppm
ppm
ppm
ppm
ppm
ppm























0
2.566
2.566
2.566
2.566
2.566
2.566
2.566
2.566
2.566
2.566
2.566
2.566
2.566


15
3.656
3.062
2.602
3.472
3.458
3.221
3.563
3.032
3.507
3.453
3.25
3.664
2.607


30
3.435
3.045
3.18
3.265
2.569
2.966
3.403
3.077
3.343
3.497
3.367
3.681
2.772


45
2.957
3.113
2.899
3.178
2.603
2.302
3.309
3.096
3.465
3.259
2.562
3.111
2.851


60
2.973
2.615
2.759
3.008
2.74
2.111
3.434
3.003
3.302
3.256
2.459
3.89
2.87


75
3.017
2.731
2.952
3.053
2.86
2.613
3.525
2.923
2.809
3.218
2.662
3.439
3.033


90
3.383
2.772
3.113
3.157
2.946
3.038
3.561
2.831
3.089
2.958
3.024
3.621
3.027


105
3.752
3.217
3.455
3.389
3.347
3.315
3.683
3.022
3.324
3.157
3.184
3.701
3.158


120
3.906
3.303
3.499
3.548
3.502
3.427
3.72
3.136
3.472
3.526
3.338
3.873
3.073


135
4.046
3.438
3.593
3.654
3.626
3.614
3.628
3.256
3.484
3.617
3.493
4.006
3.136


150
4.389
3.473
3.759
3.869
4.049
3.711
4.15
3.33
3.799
3.896
3.697
4.106
3.236


165
5.05
3.639
4.169
3.934
4.231
3.781
4.228
3.468
3.87
4.014
3.835
4.213
3.367


180
5.144
3.808
4.493
4.109
4.363
3.891
4.394
3.764
4.08
4.127
3.944
4.364
3.665
















TABLE 10







Para-anisidine value of palm oil at 50° C.






















sample
Sample
Sample
Sample
Sample
Sample
PRESOL
Sample
Sample
Sample
Sample
PRESOL




A at
B at
C at
D at
E at
F at
at
C at
D at
E at
F at
at



Control
200
200
200
200
200
200
200
500
500
500
500
500


Day
PO
ppm
ppm
ppm
ppm
ppm
ppm
ppm
ppm
ppm
ppm
ppm
ppm























0
2.69
2.69
2.69
2.69
2.69
2.69
2.69
2.69
2.69
2.69
2.69
2.69
2.69


7
3.143
3.062
3.186
3.006
3.163
3.041
3.169
2.975
2.932
3.048
3.092
3.104
3.117


15
3.585
3.296
4.011
3.337
3.819
3.293
3.417
3.124
3.09
3.329
3.814
3.301
3.437


22
3.686
3.395
4.204
3.449
4.042
3.343
3.595
3.489
3.397
3.462
3.641
3.369
3.608


30
4.545
3.74
5.542
4.033
4.62
4.036
4.121
3.95
3.782
4.066
4.546
4.089
4.273


37
5.062
4.052
5.617
4.303
4.886
4.104
4.694
4.266
4.144
4.337
4.911
4.208
4.727


45
6.054
4.209
5.794
4.636
5.502
4.433
4.771
4.455
4.249
4.606
5.271
4.589
5.085


52
6.41
4.685
5.827
4.835
5.475
4.788
5.075
4.806
4.716
4.807
5.397
4.809
5.121


60
6.942
5.091
6.165
5.079
5.681
4.96
5.205
4.92
4.822
5.137
5.614
5.052
5.155


67
7.035
5.208
6.22
5.423
5.798
5.385
5.674
5.12
4.975
5.501
5.775
5.365
5.639


75
7.29
5.514
6.269
5.271
5.789
5.233
5.417
5.271
5.089
5.3
5.862
5.35
5.454


82
7.36
5.601
6.503
5.942
5.98
5.773
5.996
5.411
5.225
5.877
5.949
5.88
6.118


90
7.676
5.827
6.657
5.956
6.092
5.866
6.048
5.818
5.521
6.047
6.074
5.993
6.096









Tables 9 and 10 illustrates the para-anisidine value of palm oil with PRESOL, TBHQ, BHA, pulverized green tea extract, crude green tea extract, cryogrinded green tea extract, rosemary extract. From the tables it can be observed that the para-anisidine values are within the threshold limits (10 meq of O2/Kg oil). This is because, para-anisidine values reflects secondary oxidation of oil and since primary oxidation would still be under process, hence secondary oxidation products would not be formed and thereby the para-anisidine values are within the limit.









TABLE 11







Totox value of palm oil at ambient temperature






















sample
Sample
Sample
Sample
Sample
Sample
PRESOL
Sample
Sample
Sample
Sample
PRESOL




A at
B at
C at
D at
E at
F at
at
C at
D at
E at
F at
at



Control
200
200
200
200
200
200
200
500
500
500
500
500


Day
PO
ppm
ppm
ppm
ppm
ppm
ppm
ppm
ppm
ppm
ppm
ppm
ppm























0
3.497
3.497
3.497
3.497
3.497
3.497
3.497
3.497
3.497
3.497
3.497
3.497
3.497


15
5.551
4.585
4.338
5.280
5.265
5.060
5.445
4.666
5.190
4.673
4.991
5.470
4.146


30
7.540
5.879
6.561
5.175
4.615
4.845
5.338
4.818
5.157
5.534
5.305
5.628
4.471


45
8.634
6.228
8.268
5.208
5.560
4.248
5.517
5.086
5.538
6.234
4.552
5.307
4.748


60
10.019
6.157
10.827
6.919
6.408
5.934
7.582
6.731
7.194
7.042
6.490
8.092
6.376


75
10.775
6.441
12.449
8.306
8.807
7.854
9.110
6.939
7.659
8.647
8.112
9.159
6.678


90
12.403
6.400
13.181
8.427
9.617
8.279
8.907
7.241
8.332
9.267
8.352
9.195
6.738


105
15.539
6.976
14.088
8.749
10.273
8.656
9.023
7.631
8.615
9.851
8.692
9.062
7.026


120
18.232
7.122
16.114
9.018
11.154
8.857
9.245
8.137
9.004
10.753
9.070
9.787
7.225


135
20.347
7.339
19.368
9.183
11.817
9.113
9.241
8.658
8.889
11.169
9.099
9.629
7.422


150
22.002
7.916
20.994
9.466
12.991
9.286
9.953
8.934
9.424
11.998
9.347
9.839
7.683


165
26.012
8.258
26.783
9.707
13.839
9.539
10.411
9.133
9.705
13.448
9.718
10.402
7.984


180
32.567
8.614
29.993
10.567
14.297
10.188
11.404
9.828
10.335
13.701
10.380
11.278
8.666









Table 11 and FIG. 6E illustrates that control and sample B has crossed the threshold limit after 180 days as in case of peroxide value. On the other hand PRESOL at 500 ppm and Sample A at 200 ppm are performing equally.









TABLE 12







Totox value of palm oil at 50° C.






















sample
Sample
Sample
Sample
Sample
Sample
PRESOL
Sample
Sample
Sample
Sample
PRESOL




A at
B at
C at
D at
E at
F at
at
C at
D at
E at
F at
at



Control
200
200
200
200
200
200
200
500
500
500
500
500


Day
PO
ppm
ppm
ppm
ppm
ppm
ppm
ppm
ppm
ppm
ppm
ppm
ppm























0
3.655
3.655
3.655
3.655
3.655
3.655
3.655
3.655
3.655
3.655
3.655
3.655
3.655


15
15.364
5.679
12.656
5.716
8.203
4.528
7.701
5.520
5.764
8.124
4.608
7.615
5.364


30
23.737
6.967
23.957
8.454
11.242
6.553
9.454
7.230
8.542
8.780
6.472
9.170
6.500


45
31.488
7.169
30.328
9.759
12.562
7.498
11.683
8.803
9.553
11.809
7.369
10.922
7.210


60
40.404
7.750
38.442
12.365
15.590
9.239
13.475
9.336
12.755
11.563
9.257
13.644
8.028


75
77.850
10.200
76.806
14.336
25.942
9.889
15.906
10.298
14.567
18.523
9.820
15.852
10.077


90
128.903
11.581
127.563
16.856
35.701
11.295
18.157
12.261
16.494
24.761
11.362
18.354
11.256


105
107.624
12.888
108.126
17.959
31.412
13.190
19.199
13.775
17.984
25.182
12.863
18.857
12.929


120
68.077
14.074
90.702
20.048
37.103
20.125
22.902
14.702
19.243
28.990
20.016
22.468
13.833


135
56.064
14.709
76.168
21.551
42.365
21.152
25.957
15.439
21.976
31.783
20.345
23.683
14.255


150
38.068
15.300
57.420
24.276
51.629
21.786
28.796
16.699
22.753
35.399
21.239
27.223
14.912


165
28.660
16.019
29.123
35.849
56.482
27.985
41.807
17.322
34.561
55.551
26.465
40.359
16.193


180
33.658
16.617
37.118
44.062
61.906
32.742
50.931
18.821
43.321
60.041
32.369
48.888
17.146









Table 12 and FIG. 6F illustrates that control and sample B has crossed the threshold limit after 180 days as in case of peroxide value. On the other hand PRESOL at 500 ppm and Sample A at 200 ppm are performing equally.


B. Determination of Shelf Life of Sunflower Oil









TABLE 13







Estimation of Shelf life of sunflower oil










Treatment
Shelf Life (days) at 30° C.














Control SFO
46.3



Sample A at 200 ppm
171.0



Sample B at 200 ppm
87.2



Sample C at 200 ppm
137.6



Sample Dat 200 ppm
83.2



Sample Eat 200 ppm
147.8



Sample Fat 200 ppm
115.7



PRESOL at 200 ppm
117.5



PRESOL at 500 ppm
134.2



PRESOL at 1000 ppm
198.5

















TABLE 14







Peroxide value of sunflower oil at ambient temperatures






















sample
Sample
Sample
Sample
Sample
Sample
PRESOL
Sample
Sample
Sample
Sample
PRESOL




A at
B at
C at
D at
E at
F at
at
C at
D at
E at
F at
at



Control
200
200
200
200
200
200
200
500
500
500
500
500


Day
SFO
ppm
ppm
ppm
ppm
ppm
ppm
ppm
ppm
ppm
ppm
ppm
ppm























0
0.758
0.758
0.758
0.758
0.758
0.758
0.758
0.758
0.758
0.758
0.758
0.758
0.758


15
4.368
2.008
3.636
3.551
4.285
3.446
3.618
2.687
4.232
4.164
3.945
4.38
2.426


30
13.706
2.927
8.816
5.794
8.638
5.292
6.656
3.478
6.862
8.44
6.027
6.985
3.096


45
19.876
3.223
10.813
8.277
9.698
7.17
8.878
4.076
10.058
9.205
8.654
10.858
3.541


60
27.018
3.335
14.091
10.01
13.774
9.427
12.059
4.687
12.682
13.552
11.797
14.07
4.007


75
32.633
3.711
17.632
11.944
16.788
11.138
13.25
5.269
13.733
15.923
12.073
14.205
4.353


90
39.991
4.088
22.615
13.127
21.797
12.531
14.842
6.462
16.117
20.813
13.58
17.56
4.8


105
48.713
4.77
28.884
17.58
26.33
15.304
19.278
7.312
19.456
25.293
16.844
20.159
5.486


120
57.501
5.13
33.526
22.001
28.554
20.025
24.212
8.328
23.059
27.932
20.989
25.356
6.176


135
67.881
5.809
41.168
25.038
35.363
23.046
28.144
9.478
25.936
34.289
23.77
29.161
6.838


150
77.186
6.387
45.546
30.001
40.412
27.58
33.795
10.037
31.597
39.268
28.875
35.537
7.648


165
86.946
7.875
55.612
35.109
51.02
33.144
37.494
11.674
36.1
49.919
34.131
39.538
8.613


180
92.913
8.252
60.578
39.591
54.15
37.852
42.26
12.461
40.22
52.295
38.821
44.094
9.462









Table 14 and FIG. 7A illustrates that that PRESOL at 200 ppm and PRESOL at 500 ppm have better activity than Samples B, C, D, E and F. Control sample is observed to cross threshold limit within one month and other samples apart from PRESOL and sample A have crossed the threshold limit in two months. Further, PRESOL at 500 ppm is showing similar activity for preventive oxidative rancidity as compared to 200 ppm of TBHQ.









TABLE 15







Peroxide value of sunflower oil at 50° C.






















sample
Sample
Sample
Sample
Sample
Sample
PRESOL
Sample
Sample
Sample
Sample
PRESOL




A at
B at
C at
D at
E at
F at
at
C at
D at
E at
F at
at



Control
200
200
200
200
200
200
200
500
500
500
500
500


Day
SFO
ppm
ppm
ppm
ppm
ppm
ppm
ppm
ppm
ppm
ppm
ppm
ppm























0
0.807
0.807
0.807
0.807
0.807
0.807
0.807
0.807
0.807
0.807
0.807
0.807
0.807


7
6.862
1.293
6.172
3.01
4.663
2.964
3.615
2.01
3.388
4.458
3.161
3.805
1.607


15
12.413
2.49
11.596
4.483
6.079
4.456
5.065
2.892
4.89
5.865
4.645
5.472
2.631


21
16.064
5.051
15.146
7.447
8.043
7.022
8.066
6.387
7.67
7.905
7.2
8.199
5.183


30
23.001
9.989
18.486
9.431
12.125
9.556
11.001
9.053
9.722
12.034
9.656
11.413
8.456


37
29.478
12.472
23.087
15.431
15.066
12.375
17.042
10.425
15.522
14.949
12.584
17.172
9.91









Table 15 and FIG. 7B illustrates that all the samples apart from PRESOL is crossing the threshold limit within one month. Since sunflower oil is unstable at higher temperature and is more susceptible to oxidation at higher temperature, PRESOL is showing better activity in preventing oxidative rancidity of sunflower oil up to 37 days.









TABLE 16







Para-anisidine value of sunflower oil at ambient temperature






















sample
Sample
Sample
Sample
Sample
Sample
PRESOL
Sample
Sample
Sample
Sample
PRESOL




A at
B at
C at
D at
E at
F at
at
C at
D at
E at
F at
at



Control
200
200
200
200
200
200
200
500
500
500
500
500


Day
SFO
ppm
ppm
ppm
ppm
ppm
ppm
ppm
ppm
ppm
ppm
ppm
ppm























0
5.941
5.941
5.941
5.941
5.941
5.941
5.941
5.941
5.941
5.941
5.941
5.941
5.941


15
6.217
6.035
6.166
6.107
6.186
6.262
6.144
6.075
6.112
6.141
6.264
6.116
6.024


30
6.29
6.083
6.258
6.252
6.212
6.378
6.286
6.142
6.254
6.208
6.364
6.301
6.102


45
6.443
6.141
6.452
6.331
6.311
6.297
6.382
6.17
6.334
6.293
6.306
6.366
6.152


60
7.115
6.224
6.793
6.702
6.37
6.405
6.792
6.256
6.772
6.354
6.453
6.836
6.23


75
7.324
6.326
6.85
6.733
6.505
6.554
6.822
6.376
6.709
6.507
6.578
6.853
6.335


90
7.771
6.493
6.962
7.083
6.73
6.651
7.222
6.556
7.119
6.704
6.693
7.242
6.513


105
8.101
6.712
7.381
7.492
7.169
7.022
7.601
6.773
7.513
7.236
7.037
7.686
6.746


120
8.352
7.039
8.154
7.885
7.583
7.729
8.053
7.109
8.006
7.585
7.853
8.15
7.056


135
9.794
7.482
9.748
8.106
7.859
9.22
8.532
7.567
8.126
7.819
9.234
8.551
7.538


150
10.698
7.901
10.661
9.029
8.07
8.724
9.467
7.903
9.109
8.057
8.756
9.484
7.935


165
11.13
8.408
11.013
10.605
8.633
10.551
10.85
8.534
10.652
8.613
10.692
10.904
8.466


180
13.065
8.896
12.115
10.803
9.136
10.767
11.164
9.046
10.827
9.123
10.772
11.211
8.982
















TABLE 17







Para-anisidine value of sunflower oil at 50° C.






















sample
Sample
Sample
Sample
Sample
Sample
PRESOL
Sample
Sample
Sample
Sample
PRESOL




A at
B at
C at
D at
E at
F at
at
C at
D at
E at
F at
at



Control
200
200
200
200
200
200
200
500
500
500
500
500


Day
SFO
ppm
ppm
ppm
ppm
ppm
ppm
ppm
ppm
ppm
ppm
ppm
ppm























0
6.237
6.237
6.237
6.237
6.237
6.237
6.237
6.237
6.237
6.237
6.237
6.237
6.237


7
6.511
6.334
6.439
6.435
6.483
6.262
6.374
6.384
6.453
6.444
6.285
6.403
6.348


15
7.165
6.675
6.842
6.548
6.51
6.378
6.636
6.706
6.555
6.499
6.401
6.689
6.681


21
7.926
7.026
7.347
6.623
6.608
6.297
6.742
7.068
6.688
6.54
6.338
6.805
7.05


30
8.532
7.11
7.392
6.702
6.37
6.405
6.729
7.091
6.82
6.36
6.467
6.923
7.063


37
9.28
7.503
8.035
6.733
6.505
6.554
6.792
7.383
6.781
6.492
6.62
6.897
7.383


45
10.014
7.754
8.438
7.083
6.73
6.651
7.222
7.558
7.255
6.707
6.756
7.372
7.504


52
10.775
8.016
9.162
7.492
7.169
7.022
7.698
7.697
7.509
7.149
7.104
7.841
7.538


60
11.464
8.208
9.641
7.885
7.583
7.729
8.112
7.718
7.964
7.593
7.761
8.132
7.597


67
12.435
8.506
9.748
8.693
7.859
8.924
8.85
8.097
8.724
7.813
9.014
8.793
7.949


75
13.278
8.863
10.661
9.613
9.249
9.313
9.763
8.182
9.696
9.328
9.386
9.815
8.06


82
14.388
8.945
11.013
10.605
10.109
10.551
11.195
8.526
10.63
10.084
10.692
11.275
8.38


90
15.714
9.484
12.411
11.098
11.188
11.061
11.462
9.471
11.146
11.319
11.059
11.611
9.378









Table 16, table 17 and FIG. 7C illustrates that PRESOL is having better activity when compared to oils of samples B, C, D, E and F and it is having activity similar to oil comprising TBHQ.









TABLE 18







Totox value of sunflower oil at ambient temperature






















sample
Sample
Sample
Sample
Sample
Sample
PRESOL
Sample
Sample
Sample
Sample
PRESOL




A at
B at
C at
D at
E at
F at
at
C at
D at
E at
F at
at



Control
200
200
200
200
200
200
200
500
500
500
500
500


Day
SFO
ppm
ppm
ppm
ppm
ppm
ppm
ppm
ppm
ppm
ppm
ppm
ppm























0
7.458
7.458
7.458
7.458
7.458
7.458
7.458
7.458
7.458
7.458
7.458
7.458
7.458


15
14.953
10.051
13.438
13.210
14.756
13.154
13.380
11.449
14.577
14.469
14.153
14.877
10.877


30
33.701
11.937
23.889
17.839
23.488
16.962
19.598
13.098
19.977
23.089
18.417
20.270
12.294


45
46.195
12.588
28.077
22.885
25.708
20.637
24.138
14.323
26.450
24.702
23.615
28.082
13.234


60
61.152
12.893
34.976
26.722
33.918
25.258
30.909
15.629
32.137
33.457
30.046
34.977
14.243


75
72.589
13.749
42.114
30.622
40.080
28.831
33.322
16.914
34.175
38.353
30.725
35.262
15.042


90
87.753
14.669
52.191
33.337
50.324
31.714
36.906
19.479
39.354
48.329
33.854
42.363
16.113


105
105.528
16.253
65.149
42.652
59.829
37.629
46.156
21.396
46.424
57.823
40.725
48.004
17.717


120
123.353
17.299
75.207
51.888
64.690
47.780
56.477
23.765
54.124
63.450
49.832
58.862
19.408


135
145.557
19.100
92.085
58.183
78.584
55.311
64.820
26.522
59.997
76.398
56.775
66.872
21.215


150
165.070
20.674
101.75
69.030
88.894
63.884
77.056
27.976
72.303
86.593
66.505
80.558
23.230


165
185.022
24.158
122.23
80.822
110.674
76.838
85.838
31.882
82.851
108.45
78.953
89.981
25.692


180
198.890
25.399
133.27
89.984
117.436
86.471
95.684
33.968
91.268
113.71
88.413
99.400
27.906
















TABLE 19







Totox value of sunflower oil at 50° C.






















sample
Sample
Sample
Sample
Sample
Sample
PRESOL
Sample
Sample
Sample
Sample
PRESOL




A at
B at
C at
D at
E at
F at
at
C at
D at
E at
F at
at



Control
200
200
200
200
200
200
200
500
500
500
500
500


Day
SFO
ppm
ppm
ppm
ppm
ppm
ppm
ppm
ppm
ppm
ppm
ppm
ppm























0
7.850
7.850
7.850
7.850
7.850
7.850
7.850
7.850
7.850
7.850
7.850
7.850
7.850


7
20.235
8.919
18.784
12.456
15.810
12.190
13.603
10.403
13.229
15.359
12.607
14.013
9.563


15
31.991
11.655
30.034
15.515
18.669
15.291
16.765
12.490
16.335
18.229
15.692
17.633
11.944


22
40.055
17.128
37.639
21.518
22.695
20.341
22.873
19.842
22.028
22.350
20.738
23.203
17.416


30
54.533
27.087
44.365
25.564
30.620
25.517
28.731
25.197
26.265
30.428
25.780
29.748
23.975


37
68.235
32.447
54.210
37.595
36.637
31.304
40.876
28.234
37.826
36.390
31.789
41.240
27.204


45
84.177
36.287
68.642
46.012
46.960
35.568
47.348
34.882
46.492
46.600
36.207
49.221
34.344









Table 18 and FIG. 7E illustrates that 200 ppm and 500 ppm of PRESOL is having better activity than antioxidant in samples B, C, D, E and F. Further, control is observed to cross threshold limit within one month. 200 ppm PRESOL is observed to prevent oxidative rancidity of sunflower oil up to 165 days and 500 ppm PRESOL is observed to prevent oxidative rancidity of sunflower oil up to 180 days. From this illustration, it can inferred that PRESOL concentration can be increased accordingly in order to prevent oxidative rancidity of oils, whereas the concentration of synthetic antioxidants cannot be increased over a particular limit as per the regulatory guidelines as they might cause harmful effects. For instance, TBHQ is a synthetic antioxidant, which cannot be used beyond the concentration of 200 ppm, as it is considered to be carcinogenic beyond 200 ppm. Further form the table 19 and FIG. 7F, it can be observed that the totox value of sunflower oil with PRESOL (200 ppm and 500 ppm) does not cross the threshold limit of 30 till 37 days, whereas sunflower oil with all other antioxidants (samples A, B, C, D, E, F) crosses the threshold limit by 37 days.


C. Determination of Shelf Life of Fish Oil









TABLE 20







Peroxide value of fish oil at 10° C.














Alpha Toco





Control
(Sample A1)
PRESOL



Day
Fish Oil
at 200 ppm
at 200 ppm
















0
1.74
1.74
1.74



3
2.09
2.13
1.89



6
3.26
3.33
2.73



9
4.62
4.71
3.46



12
5.39
5.41
3.97



15
6.74
6.82
4.39



18
7.69
7.84
4.85



21
8.98
9.02
5.48



24
10.06
10.32
5.74



27
11.38
12.02
6.24



30
12.97
13.01
6.68



33
15.39
15.44
7.14



36
16.98
17.16
7.72



39
18.72
18.94
8.26



42
20.63
20.86
8.63



45
24.82
25.09
9.01



48
28.63
28.71
9.45



51
34.74
33.89
9.87



54
39.42
39.01
10.23



57
44.66
44.14
10.69



60
48.95
49.22
11.57



63
48.05
50.06
12.03



66
46.82
51.22
12.84



69
45.08
50.85
13.38



72
41.86
50.13
14.05



75
39.71
49.72
14.87










Table 20 and FIG. 8 illustrates that peroxide value of control fish oil and fish oil added with alpha tocopherol (200 ppm) crosses the threshold limit of 8 meq/kg after 21 days, whereas fish oil with 500 ppm of PRESOL is does not cross the threshold limit till 39 days of storage, hence, proving PRESOL to be more powerful antioxidant than synthetic antioxidants.


D. Determination of Shelf Life of Canola Oil in the Presence of PRESOL

    • Shelf life of canola oil is analyzed upon adding 200 ppm of TBHQ (sample-A), BHA (sample-B), green tea extract with 90% polyphenol (sample-C), rosemary extract (sample-D), green tea extract after cryogenic grinding (sample-E), and PRESOL, respectively to canola oil.












TABLE 21







Sample
Shelf Life (No. Of Days)



















Control (Canola Oil)
58



Sample-A
181



Sample-B
37



Sample-C
149



Sample-D
74



Sample-E
202



PRESOL
256










From the table 21, it is illustrated that PRESOL increases the shelf life of canola oil by enhancing oxidative stability of the oil.


Example 4
Frying Cycle Analysis

Palm oil and sunflower oil with antioxidants added to it are obtained from a local refinery. Frying studies are carried out with control oil and by adding TBHQ (Sample A), BHA (Sample B), GT Pulverized (Sample C), ROS (Sample D), GT Cryo grinded (Sample E), GT Crude Extract (Sample F) and PRESOL, respectively to the oils. Experiments are carried out a concentration of 200 ppm and 500 ppm. Fresh potatoes of less reduced sugar content variety are used throughout the experiment which is purchased form a local supermarket. Oil samples are withdrawn from the fryer at the end of every day and stored at −4° C. until it is tested for quality parameters viz, total polar compounds. Polar compounds present in oil and fats are measured by column chromatography using standard method, ES ISO 8420:2012.


A. Frying Cycle Analysis of Palm Oil









TABLE 22







Total polar compounds of Palm oil


















sample
Sample
Sample
Sample
Sample
Sample
PRESOL





A at
B at
C at
D at
E at
F at
at



Control
200
200
200
200
200
200
200
Threshold


Cycle
PO
ppm
ppm
ppm
ppm
ppm
ppm
ppm
Limit



















0
6.057
6.307
6.325
6.357
6.752
6.304
6.655
6.528
27


8
10.275
9.18
9.754
9.087
11.039
8.944
9.703
8.564
27


16
17.083
13.4
15.964
12.322
15.534
12.071
13.17
10.565
27


24
21.268
17.913
19.329
15.872
17.699
15.127
16.264
13.855
27


32
26.9
23.217
25.264
20.351
23.851
19.55
23.583
15.064
27


40
31.33
28.187
30.192
27.059
30.051
26.005
28.072
18.058
27









Table 22 illustrates that palm oil with TBHQ, BHA, GT Pulverized, ROS, GT Cryo grinded and GT Crude Extract have crossed threshold limit for total polar compounds after 40th cycle except oil with PRESOL.


B. Frying Cycle Analysis of Sunflower Oil









TABLE 23







Total Polar compounds of sunflower oil


















sample
Sample
Sample
Sample
Sample
Sample
PRESOL





A at
B at
C at
D at
E at
F at
at



Control
200
200
200
200
200
200
200
Threshold


Cycle
SFO
ppm
ppm
ppm
ppm
ppm
ppm
ppm
Limit



















0
3.616
3.746
3.515
3.497
3.872
3.763
3.763
3.856
27


8
7.45
6.375
6.958
6.079
6.888
6.244
6.742
6.938
27


16
15.037
13.632
14.124
9.548
13.986
9.048
11.47
9.023
27


24
21.025
18.505
20.105
13.17
19.39
13.062
16.181
11.616
27


32
27.194
23.123
26.085
20.137
25.589
19.98
22.511
15.584
27


40
33.079
28.648
31.692
27.00
30.073
26.182
27.574
19.156
27









Table 23 illustrates that sunflower oil with TBHQ, BHA, GT Pulverized, ROS, GT Cryo grinded and GT Crude Extract have crossed threshold limit for total polar compounds after 40th cycle except oil with PRESOL.


Example 4
Effect of Particle Size on Antioxidant Activity of Vegetable Oils

Effect of particle size analysis on antioxidant activity is analysed with the help of Rancimat (Metrohm 743) which gives oxidative stability index based on the induction time (h). Rancimat analysis is carried out at two different temperature in order to set relationship between induction time and temperature of the studies.


Table 24 shows the particle size of different samples and its effect on antioxidant activity. In this, we have analyzed the particle size of samples with the help of Particle Size Analyzer (Microtrac, S3500) and its antioxidant activity with the help of Rancimat (Metrohm 743). Table 24 shows that reducing the particle size of GT extract has an impact on antioxidant activity. It is observed that when the particle size of GT is reduced, the Rancimat induction time increases which proves that the antioxidant activity increases on reduction of particle size. Further, the optimum particle size is between 5 to 10 μm at which the maximum activity is achieved.









TABLE 24







Relationship between particle size and antioxidant


activity of TBHQ (sample-A), 200 ppm of BHA (sample-B),


200 ppm of pulverized green tea extract with 90% polyphenol


(sample-C), 200 ppm of rosemary extract (sample-D),


200 ppm of green tea extract after cryogenic


grinding (sample-E), 200 ppm of crude green tea


extract and PRESOL at 200 ppm, 500 ppm and 1000 ppmn


in palm oil (PO) and sunflower oil (SFO), respectively.












Induction
Induction



Particle
Period (h) of
Period (h) of


Treatment
Size (μm)
PO at 120° C.
SFO 100° C.













Control

9.64
9.32


Sample A
Crystalline
20.93
26.82



form




Sample B
Crystalline
9.88
13.33



form




Sample C
46.48
17.95
24.03


Sample D
Dispersed
13.32
12.94



form




Sample E
12.81
20.02
25.28


Sample F
119.3
14.17
19.08


PRESOL
6.12
15.57
18.38


PRESOL
6.12
23.74
22.76


PRESOL
6.12
33.64
34.41









From table 24 and FIG. 11 it is illustrated that reducing particle size increases the solubility and aids to prevent sedimentation of the active components in oil matrix. As observed in the table, PRESOL at lower particle size is able to show better antioxidant activity thereby reducing the oxidative rancidity of the oil.


Example 6
Fortification of Tertiary Butyl Hydroquinone (TBHQ) and PRESOL

Synergism of TBHQ and PRESOL is analyzed in palm oil. If the frying industry is considered, synthetic antioxidant TBHQ is being added to the oils. However, there is a limitation of adding TBHQ i.e. not above 200 ppm, due to which frying oils cannot be used for longer frying cycles. In order to overcome this limitation, TBHQ is fortified with PRESOL and added to vegetable oils in order to increase the frying cycles which ultimately increases the shelf life of end products. Fortification of TBHQ & PRESOL is analyzed in Rancimat at different concentrations, ranging from about 50 to 200 ppm in palm oil. The below table 25 illustrates all the combination of fortification of TBHQ and PRESOL used in palm oil to illustrate maximum activity of fortified combination.


Synergism is calculated based on the below equation:







Synergism






(
%
)


=




(


IP

X





1

X





2


-

IP
o


)

-

[


(


IP

X





1


-

IP
o


)

+

(


IP

X





2


-

IP
o


)


]



[


(


IP

X





1


-

IP
o


)

+

(


IPIP

X





2


-

IP
o


)


]


×
100





Where,
IP0=Induction Period for Control Oil
IPX1=Induction Period for X1 (TBHQ)
IPX2=Induction Period for X2 (PRESOL)

IPX1x2=Induction Period for combination of X1 (TBHQ) and X2 (PRESOL)









TABLE 25







Synergism of TBHQ and PRESOL combination.















TBHQ
PRESOL
Induction
increase in






(Sample
(Sample
Time (H)
induction time

Increase


Vegetable
A)(ppm)
G)(ppm)
at
as compared to

in OSI
Synergism


Oil
X1
X2
120 C.
control (X-C)
OSI
(%)
(%)

















PO
0
0
9.08
0.00
1




Control


(C)


PO
50
0
9.57
0.49
1.054
5.12


PO
100
0
11.01
1.93
1.21
17.53


PO
200
0
14.24
5.16
1.57
36.24


PO
0
50
10.52
1.44
1.16
13.69


PO
0
100
11.36
2.28
1.25
20.07


PO
0
200
15.57
6.49
1.71
41.68


PO
200
100
31.8
22.72
3.50
71.45
205.38


PO
100
200
25.71
16.63
2.83
64.68
97.51


PO
100
100
30.05
20.97
3.31
69.78
398.10


PO
50
50
11.63
2.55
1.28
21.93
32.12


PO
200
200
29.32
20.24
3.23
69.03
73.73


PO
50
100
20.34
11.26
2.24
55.35
306.50


PO
50
200
24.09
15.01
2.65
62.31
115.04


PO
100
50
18.5
9.42
2.04
50.92
179.53


PO
200
50
22.44
13.36
2.47
59.54
102.42









Table 25 illustrates that the combination of 100 ppm of TBHQ and 100 ppm of PRESOL is showing synergistic antioxidant activity by suitably enhancing the oxidative stability of palm oil.


Example 7
Solubility of PRESOL in Sunflower Oil

Solubility of PRESOL is tested with respect to pulverized green tea extract (sample-C), green tea extract cryogrinded (sample-E) and crude green tea (sample-F) in sunflower oil. Solubility test is carried out by analyzing the settling percentage in the oil over storage. Settling is determined by analyzing the polyphenol content, which is present in the oil comprising the above mentioned samples using spectrophotometer at 540 nm.









TABLE 26







Solubility of PRESOL in sunflower oil.

















Concentration






Concentration
Concentration
of Polyphenols


Trial

of Blends in
Polyphenols
in Oil during
%
%


No
Treatments
ppm
in blends ppm
storage(ppm)
Solubility
Settling
















1
PRESOL
200
41.86
41.35
98.78
1.22


2

500
104.65
102.54
97.98
2.02


3

1000
209.3
200.85
95.96
4.04


4
Sample C
200
190
68.59
36.1
63.9


5

500
475
147.96
31.15
68.85


6

1000
950
253.175
26.65
73.35


7
Sample E
200
190
80.199
42.21
57.79


8

500
475
179.55
37.8
62.2


9

1000
950
314.45
33.1
66.9


10
Sample F
200
190
48.64
25.6
74.4


11

500
475
85.56
18.01
81.99


12

1000
950
99.37
10.46
89.54














Total





Polyphenols





%

=



Wt
.




of






std
×
10
×

Abs
.




of






sample
×
Ds
×
P
×
100


100





50






Abs
.




of






std






Where,

Ds=dilution of sample


Wt=Weight of the sample in gram


P=Purity of standard


From the table 26, it is illustrated that settling is on the higher side for green tea extract without grinding (sample-F) followed by pulverized green tea extract (sample-C) and at a lower side for green tea extract with cryogrinding (sample-E). However, PRESOL is having highest solubility percentage in the oil with very minimal settling over storage. The high solubility of PRESOl with minimal settling is directly linked to the percentage of polyphenols present in the composition.


Though Polyphenols is the active component which provides the antioxidant activity in green tea extracts, it has very poor solubility in oil. On the other hand, PRESOL with polyphenol percentage of about 30% to about 38% shows enhanced antioxidant activity with minimal settling over storage.


Example 8
Determining Solubility of PRESOL with Different Emulsifying Agents

Table 27 illustrates that PRESOL comprising Macrogoglycerol hydroxystearate is having an enhanced solubility with a percentage solubility ranging from about 95% to about 100%, with settling less than 5%









TABLE 27







Solubility of PRESOL comprising emulsifying agents



















Concentration







Concentration
Concentration
of Polyphenols


Trial

Emulsifying
of Blends in
Polyphenols
in Oil during
%
%


No
Treatments
Agent
ppm
in blends ppm
storage(ppm)
Solubility
Settling

















1
PRESOL
Macrogolglycerol
200
41.86
41.35
98.78
1.22


2

Hydroxystearate
500
104.65
102.54
97.98
2.02


3


1000
209.3
200.85
95.96
4.04


4
PRESOL
Sorbitol (glucitol)
200
41.86
27.26
65.11
34.89


5


500
104.65
66.02
63.09
36.91


6


1000
209.3
125.33
59.88
40.12


7
PRESOL
DATEM
200
41.86
33.17
79.25
20.75


8

(diacetyl tartaric
500
104.65
80.01
76.45
23.55


9

acid ester of mono-
1000
209.3
146.68
70.08
29.92




and diglycerides)


10
PRESOL
Guar gum
200
41.86
25.76
61.53
38.47


11

(Galactomannan)
500
104.65
60.94
58.23
41.77


12


1000
209.3
114.38
54.65
45.35









Example 9
Cost Advantage of PRESOL Over TBHQ

Case 9.1 with 200 Ppm TBHQ in Sunflower Oil (SFO)


Consider a fryer with oil bath capacity of 100 litres. We are using SFO as our medium of oil for frying potato chips. Rate of oil is 90− per kg. Rate of TBHQ is approx. 750− per kg. TBHQ dosage is 200 ppm, which is 0.2 gms in 1000 gms of oil i.e. 0.15 rupees per kg. So the net rate of oil will be (90+1.5)=90.15− per kg. Number of batches fried after adding 200 ppm TBHQ is 40 batches. Hence, total cost incurred per batch of frying will be, 100*90.15/40=225.375− per batch.


Case 9.2 with 200 Ppm PRESOL in Sunflower Oil (SFO)


Consider a fryer with oil bath capacity of 100 litres. We are using SFO as our medium of oil for frying potato chips. Rate of oil is 90− per kg. Rate of PRESOL is approx. 2500− per kg. PRESOL dosage is 200 ppm, which is 0.2 gms in 1000 gms of oil i.e. 0.5 rupees per kg. So the net rate of oil will be (90+0.5)=90.5− per kg. Number of batches fried after adding 200 ppm PRESOL is 62 batches. Hence, total cost incurred per batch of frying will be, 100*90.5/62=146.97− per batch.


Cost saved is about rupees78− (Approx. 35% reduction per Batch).


Case 9.3 with 200 Ppm TBHQ in Palm Oil (PO)


Consider a fryer with oil bath capacity of 100 litres. We are using PO as our medium of oil for frying potato chips. Rate of oil is 50− per kg. Rate of TBHQ is approx. 750− per kg. TBHQ dosage is 200 ppm, which is 0.2 gms in 1000 gms of oil i.e. 0.15 rupees per kg. So the net rate of oil will be (50+0.15)=50.15− per kg. Number of batches fried after adding 200 ppm TBHQ is 40 batches. Hence, total cost incurred per batch of frying will be, 100*50.15/40=125.375− per batch.


Case 9.4 with 200 Ppm PRESOL in Palm Oil (PO)


Consider a fryer with oil bath capacity of 100 litres. We are using PO as our medium of oil for frying potato chips. Rate of oil is 50− per kg. Rate of PRESOL is approx. 2500− per kg. PRESOL dosage is 200 ppm, which is 0.2 gms in 1000 gms of oil i.e. 0.5 rupees per kg. So the net rate of oil will be (50+5)=50.5− per kg. Number of batches fried after adding 200 ppm PRESOL is 72 batches. Hence, total cost incurred per batch of frying will be, 100*50.5/72=70.14− per batch.


Cost saved is about rupees 55− (Approx. 44% reduction per Batch).


Although cost is a relative parameter which changes with time, the costs showcased herein are applicable in August 2013, and are presented to provide an idea of the cost differential between the composition of the instant invention and the most used sample, TBHQ. This relative differential will remain the same

Claims
  • 1. A composition comprising green tea extract and rosemary extract, optionally along with adjuvant or excipient or a combination thereof.
  • 2. The composition as claimed in claim 1, wherein said green tea extract is at a concentration ranging from about 24% w/w to about 80% w/w.
  • 3. The composition as claimed in claim 1, wherein said rosemary extract is at a concentration ranging from about 45% w/w to about 85% w/w.
  • 4. The composition as claimed in claim 1, wherein said rosemary extract comprises rosemarinic acid at a concentration ranging from about 0.5% w/w to about 10% w/w and carnosic acid at a concentration ranging from about 1.0% w/w to about 20% w/w.
  • 5. The composition as claimed in claim 1, wherein the adjuvant is selected from a group comprising vitamin C, gallic acid, vitamin E, rosmanol, ferulic acid, citric acid, mixed-tocopherol, lecithin, carotenoids and uric acid or any combination thereof.
  • 6. The composition as claimed in claim 1, wherein the excipient is selected from a group comprising granulating agent, binding agent, lubricating agent, disintegrating agent, sweetening agent, glidant, anti-adherent, anti-static agent, surfactant, coating agent, colouring agent, flavouring agent, plasticizer, suspending agent, additive, emulsifying agent and spheronization agent or any combination thereof.
  • 7. The composition as claimed in claim 6, wherein the emulsifying agent is polyglyceride fatty acid ester; and wherein the additive is selected from a group comprising mono-di-glycerides, sorbitol, guar gum and xanthan gum or any combination thereof
  • 8. The composition as claimed in claim 5, wherein said adjuvant is at a concentration ranging from about 1.0 w/w to about 10% w/w.
  • 9. The composition as claimed in claim 6, wherein said excipient is at a concentration ranging from about 0.5% to about 5% w/w.
  • 10. The composition as claimed in claim 1, wherein particle size of the composition ranges from about 5 μm to about 10 μm.
  • 11. The composition as claimed in claim 1, wherein the composition optionally comprises polyphenols at a concentration ranging from about 30% to about 38%.
  • 12. The composition as claimed in claim 1 is oil soluble having solubility ranging from about 95% to about 100% with settling less than about 0 about 5%.
  • 13. A process of preparing the composition comprising green tea extract and rosemary extract, said process comprising acts of: a. granulating crude extract of green tea and mixing the granulated extract with the rosemary extract to obtain a mixture;b. optionally adding adjuvant or excipient or a combination thereof to the mixture; andc. passing the mixture of step a) or b) through homogenizer to obtain said composition comprising green tea extract and rosemary extract
  • 14. The process as claimed in claim 13, wherein the crude extract of green tea having a particle size of about 50μ to about 200μ is granulated to obtain a extract of particle size ranging from about 10μ to about 20μ.
  • 15. The process as claimed in claim 13, wherein the composition obtained in step c) has a particle size ranging from about 5μ to about 10μ.
  • 16. The process as claimed in claim 13, wherein the crude extract of the green tea is granulated by techniques selected from a group comprising hammer mill, ball mill, plate mill, disc mill, colloid mill, micronisation method, high pressure homogenization and cryogenic grinding or a combination thereof, preferably cryogenic grinding.
  • 17. The process as claimed in claim 13, wherein the mixing is carried out by an agitator at a speed of about 500 rpm to about 1000 rpm.
  • 18. The process as claimed in claim 17, wherein the mixing is at a temperature ranging from about 40° C. to about 65° C. for time period ranging from about 2 hrs to about 24 hrs.
  • 19. The process as claimed in claim 13, wherein the mixture is homogenized at a pressure ranging from about 500 bar to about 1000 bar.
  • 20. A composition comprising the composition as claimed in claim 1 and tertiary butyl hydroquinone.
  • 21. The composition as claimed in claim 20, wherein the composition of claim 1 is at a concentration ranging from about 50 ppm to about 100 ppm.
  • 22. The composition as claimed in claim 20, wherein the tertiary butyl hydroquinone is at a concentration ranging from about 50 ppm to about 100 ppm.
  • 23. An oil, fat or cosmetic preparation, comprising the composition of claim 1.
  • 24. A method of preparing the oil, fat or cosmetic preparation as claimed in claim 23, wherein said method comprises act of mixing the composition with the oil, fat or cosmetic ingredients.
Priority Claims (1)
Number Date Country Kind
3360/CHE/2012 Aug 2012 IN national
PCT Information
Filing Document Filing Date Country Kind 371c Date
PCT/IB2013/056643 8/14/2013 WO 00 3/31/2014