BEVERAGE COMPOSITIONS COMPRISING WATER-SOLUBLE PALM FRUIT BIOACTIVE COMPLEX/OIL PALM PHENOLICS AND PALM FRUIT JUICE

Information

  • Patent Application
  • 20220039421
  • Publication Number
    20220039421
  • Date Filed
    May 14, 2021
    3 years ago
  • Date Published
    February 10, 2022
    2 years ago
Abstract
The invention provides a method for enhancing flavour profile of beverages comprising increasing perceptibility of sweetness, increasing acidity, and decreasing astringent taste in beverages, increasing perceptibility of floral and spice notes by adding an effective flavour enhancing amount of water-soluble Palm Fruit Bioactive complex (wsPFBc/OPP) or their extracts into a beverage is disclosed a composition comprising a beverage and oil palm phenolics (OPP) or their extracts such that the OPP or their extracts modify or alter the fragrance and flavour of the beverage.
Description
FIELD OF INVENTION

The present invention generally relates to coffee, tea, cocoa, and other such beverage compositions such as instant tea/coffee compositions, tea leaves/coffee powder mixes, tea/coffee extracts etc that include water-soluble palm fruit bioactive complex (wsPFBc), also known as oil palm phenolics (OPP) and palm fruit juice (PFJ), for modifying or altering the characteristics of such beverages. The altered or modified characteristic is flavour and fragrance. The invention also includes the methods of preparation thereof.


BACKGROUND OF THE INVENTION

Phenolic compounds comprise an aromatic ring, bearing one or more hydroxyl substituents, and range from simple phenolic molecules to highly polymerised compounds. Despite this structural diversity, the group of compounds are often referred to as polyphenols. Most naturally occurring phenolic compounds are present as conjugates with mono- and polysaccharides, linked to one or more of the phenolic groups, and may also occur as functional derivatives such as esters and methyl esters.


Phenolic acids consist of two subgroups, i.e., the hydroxybenzoic and hydroxycinnamic acids Hydroxybenzoic acids include gallic, p-hydroxybenzoic, protocatechuic, vanillic and syringic acids, which in common have the C6-C1 structure. Hydroxycinnamic acids, on the other hand, are aromatic compounds with a three-carbon side chain (C6-C3), with caffeic, ferulic, p-coumaric and sinapic acids being the most common.


Phenolic compounds possess different biological activities, but the most important is the antioxidant activity. Their contribution to the antioxidant capacity of the human diet is much larger than that of vitamins. Current evidence strongly supports the contribution of polyphenols to the prevention of cardiovascular diseases, cancers and osteoporosis. They also play a role in the prevention of neurodegenerative diseases and diabetes mellitus.


Phenolic compounds are ubiquitous in plants, and when plant foods are consumed, these phytochemicals contribute to the intake of natural antioxidants in the human diets. Agro-industrial by-products are good sources of phenolic compounds, and have been explored as source of natural antioxidants.


Studies on flavonoids have shown that they are better antioxidants than the nutrients vitamin C, vitamin E and beta-carotene. Therefore, phenolics may be beneficial in preventing UV-induced oxygen free radical generation and lipid peroxidation, i.e. events involved in pathological states such as photoaging and skin cancer. The antioxidant properties of phenolic compounds act as free radical scavengers, hydrogen donators, metal chelators and singlet oxygen quenchers


Palm Fruit Bioactive Complex(PFBc)/Oil palm phenolics (OPP) are water-soluble antioxidants derived from the aqueous stream of palm oil milling. They contain flavonoids, polyphenols, phenolic acids, water-soluble vitamins and organic acids.


The major components in PFBc/OPP include p-hydroxybenzoic acid having a general structure as shown, and three isomers of caffeoylshikimic acid. The methyl and propyl esters of p-hydroxybenzoic acid are commonly used in the food industry as anti-microbial agents and in personal care products as preservatives.




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In the existing processes and compositions, there are relatively few existing phenolic type compounds that can the impart fragrance and taste/flavour to beverages. While beverages such as coffee and tea provide numerous health benefits, likewise wsPFBc/OPP and PFJ also provide health benefits such as preventing UV-induced oxygen free radical generation and lipid peroxidation (i.e. events involved in pathological states such as photoaging and skin cancer are absent). Given that tea and coffee being one of the largest consumed beverages, it is therefore desirable to enhance their flavour/fragrance such that they may also impart other health benefits to their existing consumer and a change in flavour/fragrance may induce more people to drink such beverages and thus promoting a healthy lifestyle.


OBJECT OF THE INVENTION

An object of the present invention is to provide edible consumable tea, coffee, cocoa or other such beverage compositions having at least one compound of water-soluble palm fruit bioactive complex (wsPFBc)/oil palm phenolics (OPP) that exhibit highly significant bioactive properties.


Another object of the present invention to provide a composition that includes a combination of phytochemical compounds from varying sources, which if added in food or beverages such as tea/coffee, can modify/improve the characteristics of said food or beverages.


Yet another object of the present invention is to provide a method for modifying or altering the fragrance and/or flavor of beverages such as tea, coffee, cocoa as combined with water-soluble palm fruit bioactive complex (wsPFBc)/oil palm phenolics.


It is further an object of the present invention to provide a composition comprising hydroxybenzoic compound(s) and other related compounds that is useful for enhancing characteristics of edible consumables.


Another object of the present invention to provide a compound, which when added in coffee, improves texture of coffee, and imparts fragrance of vanilla to coffee.


SUMMARY OF THE INVENTION

The present invention relates to a method enhancing flavour profile of beverages comprising the steps of, increasing perceptibility of sweetness, increasing acidity, and decreasing astringent taste in beverages, increasing perceptibility of floral and spice notes by adding an effective flavour enhancing amount of water-soluble Palm Fruit Bioactive complex (wfPFBc/OPP) or their extracts into a beverage.


In one aspect, beverage is coffee, particularly either a commodity coffee or a specialty coffee.


In one aspect the effective flavour enhancing amount of said polyphenols is in a concentration of about 10-80 mg/g, more preferably 20-80 mg/g or 20-40 mg/g, most preferably 30 mg/g wsPFBc in commodity coffees while 40 mg/g in specialty coffees. The flavour enhancing amount is about 3% of the whole wsPFBc and coffee beverage composition composition


The present invention further provides a method for enhancing flavour profile of coffee comprising the steps of, roasting coffee beans to produce roasted coffee beans, grinding said roasted coffee beans, preparing a coffee beverage composition, and increasing perceptibility of sweetness, increasing acidity, and decreasing astringent taste in said coffee beverage composition, increasing perceptibility of floral and spice notes by adding an effective flavour enhancing amount of water-soluble Palm Fruit Bioactive complex (wsPFBc/OPP) or their extracts into said coffee beverage composition, ground coffee beans, or roasted coffee beans.


In one aspect, the coffee beverage composition prepared may be provided as instant coffee mix, instant coffee beverage, brewed coffee, espresso, espresso-based coffee beverages, or cold brew.


In another aspect, the coffee beverage composition may be provided as ground coffee, granule mix, powder mix, powder concentrates, liquid mix, liquid concentrates





BRIEF DESCRIPTION OF THE DRAWINGS


FIG. 1—Block diagram of the raw materials used and sensory analysis steps performed.



FIG. 2—Screening of taster panel using the Wald graph.



FIG. 3.1—Evaluation of the preference of commodity (51) and specialty (S2) coffees added with wsPFBc. A: most preferred, F: least preferred. 1 (10 mg/g), 2 (20 mg/g), 3 (30 mg/g), 4 (40 mg/g), and 5 (50 mg/g).



FIG. 3.2—Influence of the addition of wsPFBc on the sensory analysis of Arabica coffee with concentrations of 0 mg/g, 10 mg/g, 20 mg/g, and 40 mg/g.



FIG. 3.3—Influence of the addition of wsPFBc on the descriptors of Arabica coffee.



FIG. 4—Sensory characteristics of commodity (51) and specialty (S2) coffees with wsPFBc added. 1 (10 mg/g), 2 (20 mg/g), 3 (30 mg/g), 4 (40 mg/g), 5 (50 mg/g), and 6 (control).



FIGS. 5a-5c—Similarity between commodity and specialty coffees in light (a), medium (b), and dark (c) roasts.



FIGS. 6a-6c—Preference and characterization of commodity and specialty coffees after light (a), medium (b), and dark (c) roasting.





DETAILED DESCRIPTION OF THE INVENTION

The following description includes the preferred best mode of one embodiment of the present invention. It will be clear from this description of the invention that the invention is not limited to these illustrated embodiments but that the invention also includes a variety of modifications, and embodiments thereto. Therefore, the present description should be seen as illustrative and not limiting. While the invention is susceptible to various modifications and alternative constructions, it should be understood, that there is no intention to limit the invention to the specific form disclosed, but, on the contrary, the invention is to cover all modifications, alternative constructions, combinations, and equivalents falling within the spirit and scope of the invention as defined in the claims.


In any embodiment described herein, the open-ended terms “comprising,” “comprises,” and the like (which are synonymous with “including,” “having” and “characterized by”) may be replaced by the respective partially closed phrases “consisting essentially of,” consists essentially of,” and the like or the respective closed phrases “consisting of,” “consists of”, and the like.


As used herein, the singular forms “a,” “an,” and “the” designate both the singular and the plural, unless expressly stated to designate the singular only.


In the following description, numerous specific details are set forth in order to provide a thorough understanding of the invention. However, it will be understood by those or ordinary skill in the art that the invention may be practiced without these specific details. In other instances, well known methods, procedures and/or components have not been described in detail so as not to obscure the present embodiment.


The present invention relates to food and beverage compositions for modifying or altering the fragrance, taste and/or flavour of food and/or beverages, comprising water-soluble palm fruit bioactive complex (wsPFBc)/oil palm phenolics (OPP) extracts.


The present invention further relates to methods of improving, modifying or altering the fragrance, taste and/or flavour of food and/or beverages flavour profiles of beverages or beverage compositions comprising water-soluble palm fruit bioactive complex (wsPFBc)/oil palm phenolics (OPP) extracts.


Water-soluble palm fruit bioactive complex (wsPFBc), also called oil palm phenolics (OPP) extracts, is herein referred as to the collective water-soluble phenolic compounds and bioactives of oil palm which is derived from the aqueous waste stream of the palm oil milling process. The wsPFBc/OPP is distinguished from the lipid-soluble bioactives or fat-soluble phytonytrients and/or bioactives of oil palm which is comprised primarily within the main product of the palm oil milling process, the crude palm oil (CPO).


The wsPFBc/OPP is comprised of water-soluble polyphenols such as phenolic acids and other compounds and bioactives of oil palm. Said wsPFBc/OPP may comprise the following major phenolic acids, water-soluble compounds, or water-soluble bioactives found in the aqueous waste stream of the palm oil milling process such as phenolic compounds, and shikimic acid. Phenolic compounds encompassing said wsPFBc/OPP may include, but not limited to caffeoylshikimic acid, caffeoylshikimic acid isomers such as 3-O-caffeoylshikimic acid, 4-O-caffeoylshikimic acid, and 5-O-caffeoylshikimic acid, para-hydroxybenzoic acid (p-hydroxybenzoic acid), protocatechuic acid (PCA), and caffeic acid. Other than shikimic acid, the wsPFBc/OPP may also comprise shikimic acid derivatives.


The wsPFBc/OPP primarily relates to the water-soluble polyphenols such as phenolic acids or compounds and bioactives of oil palm which are derived from the aqueous stream of the palm oil milling process. The aqueous stream of the palm oil milling process is also known as the vegetation liquor is considered as a by-product which is usually discarded. The source of said aqueous stream is from the sterilizer condensate and centrifuge sludge of the palm oil milling process. The sterilization part of the milling process inactivates polyphenol oxidases, while polyphenols such as phenolic acids are bioactive, hence, during the sterilization part, the processed plant compounds undergo changes in function as compared to that of the naturally occurring phenolic acids.


In one embodiment, the water-soluble palm fruit bioactive complex (wsPFBc)/OPP or extracts therefrom or water-soluble polyphenols used in the food and beverage compositions of the present invention may be obtained from vegetation liquor or aqueous stream of palm oil milling.


Vegetation liquor is a by-product of the palm oil milling process which is derived from an aqueous stream which is specifically derived from the sterilizer condensate and centrifuge sludge. While said aqueous stream is often discarded as Palm Oil Milling Effluent (POME) in the whole palm oil milling process, generation of vegetation liquor amounts to 2.5-3.5 m3 for every ton of crude palm oil produced. In the first stage of the palm oil milling process, fresh fruit bunches of the oil palm tree Elaeis guineensis are sterilized using high pressure (40 psi) steam (120-140° C.) for better separation of fruit bunches. High pressure steam sterilization further inactivates enzymes that hydrolyze the oil or enzymes that cause fruit deterioration. The high pressure steam further extracts water-soluble components which are then accumulated in the sterilizer condensate. The process then proceeds to the clarification step of palm oil milling to separate the oil from oil-water-sludge emulsion, wherein the oil is then skimmed of while the sedimented fraction (centrifuge sludge) enters the so-called aqueous stream which is rich in water-soluble phenolic acids and other water-soluble non-phenolic phytonutrients as well. The extraction of the whole oil palm vegetation liquor is demonstrated in a published patents U.S. Pat. No. 7,387,802B2 and U.S. Pat. No. 8,309,145B2, where said vegetation liquor was removed of debris and residual oil using a three-phase high-speed decanter, and then passed through a series of filters to produce a phenolic-enriched filtrate which is the so-called oil palm phenolics (OPP) or water soluble Palm Fruit Bioactive complex (wsPFBc) which contains all polyphenols or plant compounds having notable biological activities. OPP further comprises soluble fibres, sugars, and shikimic acid. In the steaming of said palm oil milling process, it must be noted that the high pressure and high temperature of the steam used inactivates polyphenol oxidases, and activates phenolic acids. While there are few heat-sensitive phenolics which may have been activated, the remaining major phenolic acids that have undergone steaming have been stabilized, improved of their bioavailability, and have their bioactive properties improved (such as antioxidant activities) when compared to their naturally occurring counterparts. While raw, unprocessed, and unextracted phenolic acids and phytonutrients exist in conjugates and complexes with glycosides and proteins, the steaming process modifies the structures and functions of these phenolics which contributes to the improved bioactive properties to which no natural counterpart may be found as similarly performing.


Beverage compositions are liquid compositions that are formulated and prepared for human consumption which may be used to quench thirst, deliver nutrition, or impart health benefits when ingested. Coffee beverages which are derived from coffee bean extracts are major sources of caffeic acid, caffeoylquinic acid, isomers of caffeoylquinic acid. Coffee beverages based on coffee bean extracts have their own unique set of phenolic compounds distinct from wsPFBc/OPP or OPP extracts. Several literatures and studies has reported and confirmed that consumption of caffeoylquinic acid have reported reduced incidence of diabetes, cardiovascular disease, and cancer. Caffeoylquinic acid also comprise anti-inflammatory and antibacterial properties. Cocoa beverages, and tea beverages, which are derived from leaves of different plants, are also comprised of different sets of collective phenolic compounds that impart their own health benefits.


In one embodiment, beverage compositions used in the present invention may include, but not limited to tea beverage compositions, coffee beverage compositions, roasted, and/or cocoa beverage compositions. Said beverage compositions may be in the form of different compositions such as infusion beverage compositions, powder mixes, and/or liquid concentrate mixes. Beverage compositions in liquid forms may be spray dried or freeze dried to obtain compositions in form of a powder. The beverages compositions of the present invention may comprise a combination of wsPFBc/OPP and coffee, wsPFBc/OPP and tea, wsPFBc/OPP and cocoa, or other further combinations. In another embodiment, beverage compositions also include raw materials for the preparation of ready to drink beverages compositions which may include but not limited to roasted coffee beans, roasted coffee grounds, dried tea leaves, crushed or ground tea leaves, roasted cocoa beans, fermented cocoa beans, or cocoa nibs.


In a preferred embodiment, the beverage or beverage composition used in the present invention is a coffee beverage or a coffee beverage composition.


A coffee beverage composition is prepared by a step of roasting raw green coffee beans. Roasting green coffee beans may be roasted in a temperature range of 160-200° C., wherein a light roast, a medium roast, or a dark roast coffee beans is achieved. Roasting green coffee beans in about 6 minutes produces light roast, in about 8 minutes produces medium roast, while in about 11 minutes a dark roast.


Coffee roasting is relevant to the influence in the sensory characteristics of coffee beverages which contribute to the acidity and bitterness. Prolonged roasting time and unequal roasting of individual coffee beans contribute to decrease acidity or intensity of acidity and increase bitterness which lowers coffee quality.


Acidity is one of the attributes that differentiates commodity and specialty coffees. The lack of selection of fruits after harvest favors the mixture of defective and immature seeds, which contributes to the low acidity in commodity coffees. On the other hand, the quality of specialty coffees contributes to better acidity. Acidity also impacts the quality and is one of the attributes evaluated in cupping. The intensity of the perception of acidity increased in both coffees after the addition of wsPFBc, and this may have occurred due to its composition of hydro acids (citric, ascorbic, lactic, glycolic, fumaric, tartaric, and salicylic acids) (U.S. Pat. No. 7,387,802 B2, 2008).


The addition of wsPFBc/OPP of the present invention improves coffee quality of both high quality/high graded or low quality/low graded coffee. In one embodiment, the present invention provides a method of improving the flavor or flavor profile of coffee, particularly improving of improving the flavor or flavor profile of roasted coffee, wherein the roast is light roast, medium roast, or dark roast.


In a preferred embodiment, the addition of wsPFBc/OPP improves the flavor or flavor profile of medium roasted coffee.


Food compositions described herein may include, but not limited to, chocolates, chocolate-based food.


A “commodity coffee” are either raw green coffee beans or roasted coffee beans wherein intrinsic coffee quality is not regarded, graded, or evaluated by a coffee grading association such as the Specialty Coffee Association.


A “specialty coffee”, also called specialty grade coffee, is regarded as raw coffee beans or roasted coffee beans to which have positive flavor attributes and profiles which are evaluated and determined by tasting or conducting sensory analysis. Specialty coffee are high quality coffee and have very minute or no defects at all in terms of coffee bean quality and taste profile.


The methods of the present invention preparation of coffee beverages or coffee beverage compositions, the preparations may be in the form of instant coffee mix, instant coffee beverage, brewed coffee, espresso, espresso-based coffee beverages, cold brew, or any related coffee beverage preparation that is known to a person of ordinary skill in the art.


The preparation of coffee beverages or coffee beverage compositions may be provided as ground coffee, granule mix, powder mix, powder concentrates, liquid mix, liquid concentrates, or any related form that is known to a person of ordinary skill in the art.


The present beverage compositions may further include flavour enhancers.


In an embodiment, the caffeoylshikimic acid extracts from water-soluble palm fruit bioactive complex (wsPFBc)/OPP are added and/or mixed with beverages to produce the beverage compositions as disclosed herein. In another embodiment, the isomers of caffeoylshikimic acid, derived from water-soluble palm fruit bioactive complex (wsPFBc)/OPP, are added and/or mixed with the beverages to produce the beverage compositions as disclosed herein. In another embodiment, the OPP extracts including caffeoylshikimic acid are added to instant beverage compositions or mixes such as instant coffee mixes.


The addition of water-soluble palm fruit bioactive complex (wsPFBc)/OPP extracts imparts additional anti-oxidant properties to the coffee or other such beverages. The palm fruit bioactives, caffeoylshikimic acid from oil palm, and caffeoylquinic acid which is a major polyphenol in coffee bean extracts share a similar pathway, and thus when brought together through such compositions as described above, provide synergistic advantages/benefits.


In one embodiment, the compositions and methods of the present invention provides a combination of caffeoylshikimic acid from oil palm and caffeoyquinic acid from coffee which consequentially provide a synergistic effect in the antioxidant activity and health benefits provided by the present invention.


The adding of water-soluble palm fruit bioactive complex (wsPFBc)/OPP to coffee or cocoa or green coffee bean extract or coffee/cocoa beverages improves taste, mouth feel, aroma, reduces bitterness, and provides additional health benefits that prevent or help in regulating major diseases and metabolic disorders such as diabetes mellitus, neurological disorders, Alzheimer's, cancer, and cardiovascular diseases among others.


The beverage composition of the present invention provides a use for modifying or altering the fragrance, taste and/or flavour of food and/or beverages. In one embodiment, the invention provides a use for improving or altering the taste and/or flavour of acidic food and/or beverages. In a preferred embodiment, the invention provides a use for improving the taste of acidic and/or bitter food and/or beverages compositions.


The beverage compositions or coffee compositions provided herein may further comprise sweeteners such as stevia or sugar.


In a further embodiment, the beverages also include tea from Camellia sinensis, or Ginseng tea, herbal tea, or a combination thereof.


In humans, bitter receptors (hT2receptorRs) are encoded by 25 different bitter receptor genes. The water-soluble palm fruit bioactive complex (wsPFBc)/OPP serve as bitter receptor antagonists that mask bitterness that is tasted in coffee, tea, or cocoa beverage compositions. Said receptor antagonists found in OPP are phenolics and oligosaccharides. Furthermore, p-hydroxybenzoic acid, an OPP, is a known as a flavor enhancer.


In an embodiment, the water-soluble palm fruit bioactive complex (wsPFBc)/OPP contains glucose, fructose, sucrose and these may further modulate bitter taste in food and/or beverages. OPP is high in potassium which presumably imparts a salty taste and this too could mask the bitterness.


In one embodiment, a method for improving the flavour of a food and/or beverage composition is provided.


In one embodiment, the present invention further provides a method for enhancing flavour profile of beverages further comprising a step of adding extracts from a Cannabis plant and/or synthetic cannabinoids which further contributes to the improvement of flavour of beverages. Extracts from Cannabis plant may be derived using High Performance Liquid Chromatography (HPLC). Extracts from Cannabis plant and/or synthetic cannabinoids elicit health benefits or numerous therapeutic effects which includes, but not limited to antioxidant activity, reduction of inflammation, pain reliever, and anti-proliferative effects. While the use of cannabinoids may be therapeutic, its combination along with caffeoylshikimic acid from oil palm, and caffeoylquinic acid from coffee provides a synergistic effect towards the provision of a beverage composition with health benefits, more particularly a synergistic antioxidant effect when combined in a beverage composition.


Sensory Perception of Commodity and Specialty Coffees

Sensory tests were conducted wherein samples were coded with three digits and presented at random. Approximately 30 ml of each sample was offered to the tasters in 50 ml plastic cups. Participants were instructed to rinse their mouths with water between samples to clean the palate. The samples used, degree of roasting, wsPFBc concentration, and stages of sensory analysis are described in FIG. 1.


Selection of Tasters

Coffee consumers (20 in number) were invited to participate in the sensory analysis on a voluntary basis. From the triangular test, 7 tasters were selected because they could discriminate samples of commercial coffees with and without the addition of wsPFBc (3%) (Meilgaard, Civille, & Can, 1999). The results were statistically evaluated using Wald's sequential analysis, according to the graphical method (Amerine, Pangborn, & Roessler, 1965). The Wald graph was constructed based on the parameters P=0·30, p1=0·66, α=0·10, and β=0·05. Further, the judges were selected or rejected according to the number of correct answers (FIG. 2).


In one embodiment, wsPFBc is added in commodity coffee or specialty coffee to produce a beverage composition with enhanced, improved, or modified flavor, that is a coffee beverage composition, wherein said desired beverage composition comprises of about 1-5% wsPFBc/OPP, about 1-4% wsPFBc/OPP, about 1-3% wsPFBc/OPP, about 2-3% wsPFBc/OPP, or about 3% wsPFBc/OPP.


Training Session

The selected tasters were trained to recognize basic tastes that are sweet, sour, and salty, following the recommendations of the Coffee Quality Institute. Three differently tasting solutions with different concentrations were prepared. These were saline (0.1, 0.2, and 0.3%), sweet (0.75, 1.5, and 2.25%), and acidic (0.15, 0.3, and 0.45%). The solutions were presented separately in each session, for the recognition and differentiation of concentrations. After this stage, the solutions were combined in different proportions, and the tasters were asked to identify the basic tastes present in each mixture. The sessions were repeated until all participants were able to discriminate all solutions.


The intensity analysis was conducted after training. The tasters were instructed to taste the coffee samples added with wsPFBc and indicate how much more or less acidic it was than the control (without wsPFBc). The sensory evaluation form was based on a 9 cm unstructured linear scale, anchored at its ends with terms that expressed intensity. When the attribute had the possibility of being equal to the control, the middle of the scale was marked. Besides, they were asked to order the samples according to preference from most preferred to least preferred.


Determination of the Concentration of wsPFBc Added


The sorting task was carried out to group the samples in terms of acidity and determine the best concentrations of PFBc to be added in commodity and specialty coffees. The trained tasters received samples with and without the addition of PFBc in concentrations of 10, 20, 30, 40, and 50 mg/g. Further, they were instructed to group the 12 samples by similarity and describe them according to acidity. The data were subjected to analysis of variance (ANOVA), and the means were compared based on the Scott-Knott test (p<0.05) using the SISVAR software from Ferreira (2014).


In one embodiment, the addition of wsPFBc/OPP in either commodity or specialty coffees may be added in various forms such as dried solids, spray-dried wsPFBc/OPP, freeze-dried wsPFBc/OPP, granules, powders, liquid concentrates, liquids, and other forms known to a person of ordinary skill in the art which may be applied to modification of flavor of beverage compositions. Preferably, the added wsPFBc is in solid form as dried solids, granules, or powders.


Training and Descriptive Analysis of Coffee

Commodity and specialty coffees of the Catuaí red variety processed by the natural (83 and 85 points—SCA scale) and pulped natural (82 and 88 points) methods were subjected to three roasting profiles, namely, light, medium, and dark. The sensory descriptors of the coffees in each roasting profile were defined in a round table testing by three certified Q-grader tasters. The main descriptors included flavors profile and attributes such as citric acid, malic acid, woody, bitter, almonds or nuts, peanuts, caramel, black tea, bitter chocolate, milk chocolate, light-body, heavy-body, spices, phenolic, floral, fruity, yellow fruits, dried fruits, herbaceous, honey, dairy notes, coffee pulp, burnt, rancid, brown sugar, tobacco, and wine. After this stage, the seven tasters were trained to describe the coffee's attributes through the recognition of the described characteristics.


The chosen method with 8% coffee was used to prepare the beverage with and without the addition of PFBc. The concentrations of the bioactive complex were selected according to the taste preferences of commodity and specialty coffees. Further, the sorting task was used to group the 10 coffee samples by similarity and preference and carried out in two sessions for each roasting profile. Additionally, the tasters were instructed to describe the main sensory characteristics of each group. The data were statistically analyzed by employing the Multiple Factor Analysis (MFA) using XLSTAT.









TABLE 1







Sample Identification.













Roast












Treatment
Processing
Quality
Light
Medium
Dark





Control
Natural
Commodity
611
612
613



Pulped
Specialty (85 pts)
621
622
623



Natural
Specialty (82 pts)
631
632
633



Pulped
Specialty (83 pts)
641
642
643



Natural
Specialty (88 pts)
651
652
653



Natural
Commodity

667
663


PFBc
Natural
Commodity
411
412
413



Pulped
Specialty (85 pts)
421
472
423



Natural
Specialty (82 pts)
431
432
433



Pulped
Specialty (83 pts)
441
442
443



Natural
Specialty (88 pts)
451
452
453



Natural
Commodity

462
463










Selection of wsPFBc Concentration in Coffee


The influence of the addition of the palm fruit bioactive complex (PFBc) on the sensory profile of commodity and specialty coffees was evaluated in this work. The addition of the bioactive complex was shown to influence acidity at different intensities (data not shown) according to the coffee quality. The PFBc concentrations of 30 and 50 mg/g significantly influenced the sample of commodity coffee, and in the sample of specialty coffee, the concentrations of 30, 40, and 50 mg/g showed a significant difference (Table 2). Averages of intensity of acidity were shown in Table 2 and were derived using the Scott-Knott test at 5% probability.









TABLE 2







The intensity of acidity correlated


with PFBc concentrations added to coffee









PFBC




(mg/g)
Commodity
Specialty





10
 5.04b
5.64b


70
 5.72b
5.62b


30
 6.05a
6.69a


40
5.3b
6.49a


50
 6.87a
6.56a









From the preference analysis, the concentrations of 30 mg/g and 40 mg/g were selected for commodity and specialty coffees, respectively (FIG. 3.1). In these concentrations, the addition of wsPFBc increased the acidity of the drinks Commodity coffee had low acidity, whereas specialty coffees had a high acidity (FIG. 4). Furthermore, the addition of 40 mg/g of wsPFBc on the sensory profile of Arabica coffees showed an excellent perception of sweetness, acidity, aftertaste, and less astringency (FIG. 3.2). Noticeable floral and spice notes were observed in 20 mg/g and 40 mg/g wsPFBc added Arabica coffee while fruity and sour/fermented notes were perceived more intensely at the concentration of 40 mg/g (FIG. 3.3). It is further emphasized that the enhancement and modification of the coffee beverages using wsPFBc has increased perception of sweetness, which is contrary to the common improvement of flavor by addition of sugar components which only increases sugar content which is a major problem for consumers that have compromised health, particularly coffee drinkers which body and digestion that is not able to process sugars.


In FIG. 3.1 where different commodity and specialty coffees, which were added with wsPFBc, were scored and graded by the standardized coffee tasters or coffee Q-graders following the Specialty Coffee Association protocols and methodologies for grading coffee. The addition of 40 mg/g of wsPFBc in specialty (S2) coffee was the most preferred (preference A) while the addition of 10 mg/g and 30 mg/in commodity coffee (S1) was the next most preferred (preference B).


In FIG. 4 where sensory characteristics were assessed, specialty coffees (S2) with 40 mg/g and 50 mg/g added wsPFBc were determined to have high acidity while commodity coffee (S1) with added 10 mg/g and 30 mg/g were determined to have low acidity.


Acidity is important in the overall quality of the coffee with consequently affects evaluation during coffee cupping, as well as perception of acidity. While commodity coffee are often classified as low quality due to their loss of acidity, the primary cause may be pointed to lack of quality fruit selection after harvest, lack of selection of mature seeds, and lack of quality control in removing defective seeds. In these cases, the perception of acidity, as well as the acidity of coffee is not given well by commodity coffee. The increase in the perception of acidity for both commodity and specialty coffee may have been due to the composition of the added wsPFBc which comprises organic acids such as citric acid, ascorbic acid, lactic acid, glycolic acid, fumaric acid, tartaric acid, and salicylic acid.


Gas Chromatography—Mass Spectrometry (GC-MS) Analysis

The analysis of volatile compounds was performed in commodity and specialty coffees medium roasting at the following concentrations of PFBc: 0, 10, 20, 30, 40, and 50 mg/g. The volatile compounds of the PFBc matrix were also evaluated. Volatile compounds were extracted using manual Headspace-solid phase microextraction (HS-SPME) from coffee beverages. The compounds were analyzed using a Shimadzu QP2010 GC model equipped with mass spectrometry (MS) and a silica capillary Carbo-Wax 20M (30 m×0.25 mm×0.25 mm) column. The oven temperature was maintained at 60° C. for 5 min with increments of 10° C./min and then maintained at 230° C. for 15 min. Injector temperatures were kept at 230° C. in splitless mode. The volatile compounds were identified by comparing the mass spectra to the NIST11 library. 9


Also, an alkane series (C10-C40) was used to calculate the retention index (RI) for each compound and compare it with RI values found in the literature.


Commodity and specialty coffee samples submitted to GC-MS analysis differed in terms of volatile composition. From the 88 identified compounds, there were 13 acids, 8 alcohol, 2 aldehyde, 1 amide, 3 esters, 10 furans, 3 ketones, 2 lactones, 6 phenol, 2 pyranones, 2 pyrazines, 1 pyridine, and 34 others (Table 2).









TABLE 2







Volatile compound (area) of commodity and specialty coffees with wsPFBc added in different concentrations.





















Compounds
RI
PFBC
0
10
20
30
40
50
0
10
20
30
40
50
























Acid
















Propanoic acid
1518
1300064
11
37
34
27
19
41
49
35
27
43
37
36


2-Butenoic acid
1776
0
41
78
68
77
77
106
167
139
114
154
186
210


3-methyl-2-Pyridinecarboxylic acid methyl ester
1885
245
0
0
0
0
0
0
0
0
0
0
0
0


Acetic acid
1431
0
2418432
4273600
3867183
2854023
2733202
3216481
2768503
1843518
1497918
2597118
2456190
1996276


Butanoic acid
1651
201
338
666
612
519
470
920
1199352
1146323
1154580
1180351
1368455
1643821


3-methyl-Cyclohexane-carboxylic acid
1995
161
0
0
0
0
0
0
0
0
0
0
0
0


Hexadecanoic acid methyl ester
2107
24
18
28
114
44
63
26
33
34
36
37
37
55


Hexanoic acid
1816
1194638
0
85
72
75
85
194
125
100
91
192
150
217


Decanoic acid
2171
74
0
0
0
0
0
0
0
0
0
0
0
0


Nananoic acid
2067
117
21
48
46
27
45
56
59
41
42
51
44
76


Octanoic acid
1958
218
11
28
30
24
44
48
44
22
34
35
23
61


Pentanoic acid
1723
3455426
7
34
24
22
27
41
21
21
24
45
48
76


4-hydroxyphenyl phosphonic acid
1895
822
1645697
2380356
2363977
2059550
1557951
2521381
270
227
208
239
278
252


Alcohol
















1-Dodecanol
1882
110
365
96
986
257
149
67
97
62
90
89
86
111


4-Nananol
1476
8753431
0
0
0
0
0
0
2957810
853
119
553
1764725
901


Benzyl alcohol
1831
116
99
26
26
27
21
109
44
36
28
39
49
60


2-(dodecyloxy)-Ethanol
2142
0
25
26
110
52
52
26
20
18
33
21
21
33


1-Heptadecanol
2267
141
175
54
66
122
273
86
48
35
34
39
32
34


1-Heptadecanol
2268
141
175
54
65
122
273
86
48
35
34
36
32
34


1-Tridecanol
2073
9
12
10
70
29
30
11
21
16
24
18
15
21


Phenylethyl Alcohol Aldehyde
1851
139
186
224
212
237
178
503
281
198
146
218
258
341


Benzene-acetaldehyde.alpha.-ethylidene-2 Furan-
1861
14
128
167
168
145
124
192
106
83
85
91
117
157


carboxaldehyde
















5-methyl-Amide
1543
102
8185084
13221919
13145821
9541586
7937607
11839760
9829899
9145793
10953642
9282604
11086572
13602906


Acetamide Ester
1788
414
0
0
0
0
0
0
0
0
0
0
0
0


Dibutyl adipate
2162
178
25
124
91
84
94
20
100
701
353
487
493
576


Homosalate
2337
26
14
21
75
47
82
37
48
59
58
54
56
65


Isopropyl palmitate
2132
39
24
16
21
24
37
20
15
9
7
10
10
11


Furan
















2-Furanmethanol
1632
902
7137434
9788869
9281580
8384452
6592188
9691290
5393720
4727051
4387766
4757822
4987850
5391194


2-Furanmethanol acetate
1495
0
12113568
16684506
17485390
11834990
10242856
6554472
3548066
3462977
4640233
3566608
4047144
4561224


2-Furanmethanol propanoate
1558
8
1686123
1639499
1816336
1421244
1136969
608
219
261
351
224
258
291


Benzofuran 23-dihydro-
2286
24
191
205
234
266
219
288
136
102
77
107
142
184


Ethanone 1-(1H-pyrrol-2-yl)-
1882
129
855
1016797
978
1199602
893
1151084
540
390
257
418
485
556


Ethanone 1-(2-furanyl)-
1471
0
2147256
2507625
3335160
2370280
2055874
3055097
2516256
2380389
3214509
2140837
2670546
2737259


Furan 22′-[oxybis-(methylene)]bis-
1878
0
2128791
2533889
2795157
2452389
2059073
3102941
310
239
259
248
352
438


Furan 22′-methylenebis-
1562
74
1218749
378
419
213
296
333
24
29
37
27
48
15


Furan 2-[(methylthio)methyl]-
1442
52
1897181
1059051
645
889
790
566
0
0
0
0
0
0


Furfural
1417
254
5678822
2519730
8286589
2075151
1354555
9162216
12303618
6325074
11872886
12711619
1471808
11797534


Ketone
















2-Propanone 1-(acetyloxy)-
1427
0
2315066
4154653
3762138
3106031
2643767
3042131
1990027
1815768
1492676
2083044
124237
1717211


4-Hydroxy-2-methylace-topheneone
2091
157
6995429
8220536
8785776
7951264
6542514
9939825
2468047
1891763
1720490
1947355
2573375
3353271


2,5-Dimethyl-4-hydroxy-3(2H)-furanone
1950
353
48
41
34
60
35
36
103
65
20
78
72
53


Lactone
















δ-Valerolacctone
1803
210
0
0
0
0
0
0
0
0
0
0
0
0


Dehydromevalonic lactone
1945
128
0
0
0
0
0
0
0
0
0
0
0
0


Phenol
















Phenol 24-bits (11-dimethylethyl)-
2188
463
144
135
192
161
208
236
101
110
147
136
320
272


Phenol
1895
822
1665783
2380356
2363977
2059550
1557951
2521381
270
227
208
239
278
352


Phenol 2-methoxy-
1818
28
2887870
4397541
4311312
3441795
2720909
4463501
305
251
263
264
316
411


Phenol 3-methyl-
1982
6
159
213
209
195
144
252
60
45
39
47
59
79


Phenol 4-ethyl-Phenol 4 ethyl-
2070
7
253
329
322
312
247
417
44
32
29
35
46
60


2-methoxy-
1914
47
5580342
7365718
7364182
6613943
5395609
8765283
347
264
260
269
348
476


Pyranone
















2,3-dihydro-3,5-dihydroxy-6-methyl-4H-pyran-4-one
2177
946
0
106
28
0
0
0
60
47
11
89
85
31


Maltol
1889
1226903
275
487
319
384
302
263
176
131
64
144
151
134


Pyrazine
















Pyrazine 2-ethyl-3,5-dimethyl-
1458
0
1414304
2099077
745
1621287
1396079
2185738
773
638
676
645
800
1181131


Pyrazine trimethyl-Pyridine
1398
0
771
1773963
1692734
1203565
1049909
1674772
602
453
524
549
243
429


(4H)-Pyridine N-acetyl-
1684
16
1015820
1386852
1430313
1168499
977
1475792
577
457
415
481
556
680


Others
















355-Trimethylhexyl acetate 13-Dioxol-2-one
1369
601
0
0
0
0
0
0
0
0
0
0
0
0


4,5-dimethyl-16-Octadien-3-ol
2043
1688264
16
50
28
17
11
34
29
27
21
10
23
32


37-dimethyl-1H-Pyrrole-2-carboxaldehyde
1532
0
125
100
88
74
58
66
74
64
94
75
97
97


1-methyl-
1588
132
1882213
3056925
3103782
2006887
1720801
2527405
1330085
1220831
1539980
1237550
1428869
1781598


2-Thiophenemethanol
1865
0
50
59
54
60
48
65
45
31
21
34
40
44


Furfural acetone 3-Furanacetic acid 4-hexyl-2,5-dihydro-
1846
0
98
126
155
135
102
181
57
43
45
48
67
88


2,5-dioxo-4-Hydroxy-
2006
197
0
22
15
14
19
50
0
7
15
33
48
72


3-methylacetophenone 23-Bis(acetyloxy)
1905
5
181
227
272
241
199
314
68
56
54
58
77
109


butanedioicacid
1428
0
2353860
4154653
377185
3116110
2664510
3102614
1944531
1825883
1497918
897
2384873
1959941


Megastigmatrienone
2125
0
15
17
20
17
16
22
13
11
10
10
14
18


Octyl ether
1743
42

0
0
0
0
0
0
0
0
0
0
0


Oxazolidine 22-diethyl-3-methyl-
1829
86
0
0
0
0
0
0
0
0
0
0
0
0


RT:11.735
1650
601
0
0
0
0
0
0
0
0
0
0
0
0


RT:11.940
1668
0
483
603
796
558
505
912
217
167
165
182
201
294


RT:12.405
1706
0
1250931
502
533
409
348
379
259
281
366
290
379
236


RT:12.435
1709
0
421
589
577
452
366
579
45
46
47
42
56
72


RT:13.435
1792
1351502
1472823
803
1573863
698
861
1097519
221
132
153
100
179
268


RT:13.495
1797
1351502
1555220
841
1626025
698
861
1097519
239
132
153
100
178
265


RT:13.945
1820
17
791
1018073
1079509
954
803
1292403
619
473
407
507
644
914


RT:14.230
1834
3
1597193
915
908
819
610
650
197
141
174
155
185
130


RT:14.785
1862
0
170
134
224
184
148
228
0
0
0
0
0
0


RT:14.980
1871
0
266
303
363
316
227
450
167
128
118
137
171
257


RT:15.015
1873
66
0
0
0
0
0
0
0
0
0
0
0
0


RT:15.135
1879
294
0
0
0
0
0
0
0
0
0
0
0
0


RT:15.325
1888
173
333
273
441
185
607
1843245
48
29
42
29
54
158


RT:16.205
1968
109
0
0
0
0
0
0
0
0
0
0
0
0


RT:16.650
2016
64
0
0
0
0
0
0
0
0
0
0
0
0


RT:16.990
2053
22
56
55
60
85
198
475
19
14
17
14
19
127


RT:17.495
2107
24
0
0
0
0
0
0
0
0
0
0
0
0


RT:17.885
2149
90
0
0
0
0
0
0
0
0
0
0
0
0


RT:17.890
2149
90
557
659
744
717
579
922
529
407
367
427
566
754


RT:18.105
2172
0
113
157
173
184
135
230
127
125
127
120
137
186


RT:22.860
2663
17
2
8
13
6
9
3
3
16
12
13
17
23


Trisiloxane 1,1,1,5,5,5-hexamethyl-3,3-bis
1616
527
512
127
1013566
480
156
157
244
79
82
65
101
189


[(trimethylsilyl)oxy)-









2-Pyridinecarboxylic acid methyl ester; decanoic acid; acetamide; δ-valerolactone; dehydromevalonic lactone; 3,5,5-trimethylhexyl acetate; octyl ether; oxazolidine 2,2-diethyl-3-methyl-; among other non-identified volatiles (RT:11.735; RT:11.940; RT:12.405; RT:12.435; RT:13.435; RT:13.495; RT:13.945; RT:14.230; RT:14.785; RT:14.980; RT:15.015; RT:15.135; RT:15.325; RT:16.205; RT:16.650; RT:16.990; RT:17.495; and RT:17.885) were present in the Palm Fruit Bioactive complex (PFBc), However, these compounds were not detected after coffee preparation. Volatile compounds that have low molecular weight (<300 Da) which characterizes them by the rapid volatilization and were probably volatilized during the coffee extraction process.


The principal component analysis explained 74.63% of the variation in data for commodity coffee and 71.87% of the variation in specialty coffee variation. The coffees without PFBc were grouped separately from the others, showing the influence of PFBc on the volatiles profile (S1.0 and S2.0).


Ester was the group of volatiles correlated with commodity coffee added with 30 mg/g of PFBC (S1.3) represented by dibutyl adipate, homosalate, and isopropyl palmitate.


In one embodiment, the beverage composition with added wsPFBc of the present invention, particularly commodity coffee beverage compositions or commodity coffee, further comprises of volatile compounds, wherein said volatile compounds are esters selected from the group consisting of dibutyl adipate, homosalate, and isopropyl palmitate.


Specialty coffee with 40 mg/g of PFBc (S2.4) was correlated with acids and pyranone. Propanoic acid; 2-butenoic acid 3-methyl-; acetic acid; butanoic acid 3-methyl-; hexadecanoic acid methyl ester; hexanoic acid; decanoic acid; nonanoic acid; octanoic acid; pentanoic acid; and 4-hydroxybenzenephosphonic acid were present in coffee, and their concentration has changed with the addition of PFBc. High acidity was noticeable by the tasters and was probably influenced by the intensity of the volatile acids. Acetic acid, butanoic acid, and hexanoic acid have been reported as the main volatile acids that influence coffee acidity. Propanoic acid causes off-flavor to the coffee beverage and addition of wsPFBc in coffee reduced propanoic acid content by 24.8% when compared with coffee without wsPFBc.


In one embodiment, the beverage composition with added wsPFBc of the present invention, particularly specialty coffee beverage compositions or specialty coffee, further comprises of acids and pyranone, selected from the group consisting of propanoic acid; 2-butenoic acid 3-methyl-; acetic acid; butanoic acid 3-methyl-; hexadecanoic acid methyl ester; hexanoic acid; decanoic acid; nonanoic acid; octanoic acid; pentanoic acid; and 4-hydroxybenzenephosphonic acid.


The medium-chain fatty acids such as nonanoic acid, octanoic acid, decanoic acid, and pentanoic acid contribute to the overall volatile profiles, conferring on them moderate and pleasant notes.


Pyranones are generated from sugar fragmentation of deoxyosones, resulting in 2,3-dihydro-3,5-dihydroxy-6-methyl-4H-pyran-4-one, and maltol imparting a caramel aroma to the beverage can contribute to antioxidant capacity.


Influence of wsPFBc on Coffees of Different Qualities


The bioactive complex of palm fruit extract is rich in phenolic compounds that, in addition to having antioxidant properties, are characterized as aromatic metabolites, contributing to changes in the sensory profile of the final product. The perception of PFBc in the coffee was evident in the medium roasted variants, followed by light and dark roasted coffees. At each stage of the roasting process, the sensory characteristics of coffee beans were modified due to changes in the concentrations of volatile and non-volatile compounds present in the beans. In the light roast (FIG. 5), natural coffee classified at 88 points was the type one that showed no difference in sensory characteristics after the addition of wsPFBc and was grouped in the negative component (F2).


Among the roasting profiles, FIG. 6 shows the preferences and characterization of the coffee roast profiles under light roast (6a), medium roast (6b), and dark roast (6c). The medium roast is considered ideal because it has a balance between flavor and aroma, contributing to a full beverage with an intense citrus flavor compared to other roasts according to literatures. In this roasting profile, specialty coffees with scores below 85, such as coffees processed by the natural (82 pts) and pulped (83 pts) methods, showed greater acceptance after the addition of wsPFBc. Despite being classified as “very good” coffees (80-84.99), the reduced complexity of aroma and flavor when compared to coffees with higher scores allowed a better performance of wsPFBc, contributing to an increase in the body.


The addition of wsPFBc was less noticeable in coffee with a dark roast. Control pulped (83 and 85 pts), and commodity coffees with wsPFBc showed a different profile. The pulped (83 pts) and natural (82 and 88 pts) control coffees were the most preferred. These coffees were characterized by the flavor of almonds and nuts, milk chocolate, and brown sugar (FIG. 6).

Claims
  • 1. A method for enhancing flavour profile of beverages comprising: (A) increasing perceptibility of sweetness, increasing acidity, and decreasing astringent taste in beverages, and(B) increasing perceptibility of floral and spice notes by adding an effective flavour enhancing amount of water-soluble Palm Fruit Bioactive complex (wfPFBc/OPP) or their extracts into a beverage.
  • 2. The method of claim 1, wherein said beverage includes coffee.
  • 3. The method of claim 2, wherein said coffee is commodity coffee.
  • 4. The method of claim 2, wherein said coffee is specialty coffee
  • 5. The method of claim 1, wherein said effective flavour enhancing amount is in a concentration of 20-80 mg/g.
  • 6. The method of claim 5, wherein said effective flavour enhancing amount is added in an amount of approximately 3% of the beverage.
  • 7. The method of claim 1, wherein said effective flavour enhancing amount is in a concentration of 30-40 mg/g.
  • 8. The method of claim 7, wherein said effective flavour enhancing amount is added in an amount of approximately 3% of the beverage.
  • 9. The method of claim 3, wherein said effective flavour enhancing amount is added to the commodity coffee at 30 mg/g concentration.
  • 10. The method of claim 9, wherein said effective flavour enhancing amount is added in an amount of approximately 3% of the beverage that includes the commodity coffee.
  • 11. The method of claim 4 wherein said effective flavour enhancing amount is added to the specialty coffee at 40 mg/g concentration.
  • 12. The method of claim 11, wherein said effective flavour enhancing amount is added in an amount of approximately 3% of the beverage that includes the specialty coffee.
  • 13. A method for enhancing flavour profile of coffee comprising: roasting coffee beans to produce roasted coffee beans;grinding said roasted coffee beans;preparing a coffee beverage composition using the roasted coffee beans;increasing perceptibility of sweetness, increasing acidity, and decreasing astringent taste in said coffee beverage composition, and increasing perceptibility of floral and spice notes by adding an effective flavour enhancing amount of water-soluble Palm Fruit Bioactive complex (wsPFBc/OPP) or their extracts into said coffee beverage composition, ground coffee beans, or roasted coffee beans.
  • 14. The method of claim 13, wherein the prepared coffee beverage has the form of at least one of: ground coffee, a granule mix, a powder mix, powder concentrates, a liquid mix, and liquid concentrates.
  • 15. The method of claim 13, wherein the prepared coffee beverage composition is provided as at least one of: an instant coffee mix, an instant coffee beverage, brewed coffee, espresso, espresso-based coffee beverages, and cold brew.
  • 16. The method of claim 15, wherein the prepared coffee beverage composition has the form of at least one of: ground coffee, a granule mix, a powder mix, powder concentrates, a liquid mix, and liquid concentrates.
Provisional Applications (2)
Number Date Country
63025097 May 2020 US
63025090 May 2020 US