Patent Application
20050186235
The present disclosure provides cosmetic compositions for making up and/or caring for the skin, such as the face.
The compositions disclosed herein may be used in makeup products, for example, for the face, and may have non-therapeutic care and/or treatment properties. They may be “matting” cosmetic compositions, i.e., compositions intended to reduce the sheen of greasy skin and/or to improve the long-term staying power of makeup, i.e., to prevent visual degradation in the course of the day.
Many makeup compositions of this type are in the form of compact powders generally comprising a fatty phase, conventionally known as a “binder,” and a pulverulent phase comprising pigments and/or fillers. The main function of the binder is to ensure sufficient cohesion of the final composition, i.e., to prevent its fragmentation, which may be caused by impacts, and to give it a good capacity to be taken up.
For these properties to be obtained, the other components of the cosmetic compositions, including the fillers they contain, also should be suitable for placing in a compact powder form.
However, certain fillers lack the ability to be compacted. These are referred to as “incompactable” fillers. Consequently, their presence in a cosmetic composition intended to be formulated in compact powder form may significantly affect the cohesion of the resulting powder, or even, when they are in large amount, make it impossible to obtain a corresponding compact powder using a mechanical press.
Low-density fillers may also raise a problem for the formulation of compact powders having satisfactory cohesion and/or cake-erosion characteristics. Thus, when such a filler is present in an excessive content, generally of greater than or equal to 5% by weight relative to the total weight of a composition intended to be compacted, it cannot be compacted satisfactorily with a standard binder such as isocetyl stearate or with the silicone binder described in patent application WO 93/17660, used at low content, for example, from about 3% to 5% by weight. However, increasing the binder content to improve the compacting, for example to a scale of 10% by weight of binder in the composition, generally proves to be detrimental to the surface appearance, which is then too greasy. Furthermore, the high cohesion thus obtained makes it difficult to erode the composition using an applicator such as a powder puff, brush, and even a finger.
Another alternative is disclosed in EP 0 717 979. This alternative comprises preparing “compact” powders from about 30% by weight of “incompactable” fillers, about 5% by weight of liquid binder and more than 50% of water, via a freeze-drying technique. However, this freeze-drying process can be a laborious technique to implement industrially, for instance, since it requires freezing of the intermediate composition.
There is thus a need for compact powder cosmetic compositions, which, although comprising large amounts of incompactable fillers and/or low-density fillers, nevertheless can have satisfactory cohesion and/or erosion properties, and are moreover not restricting in terms of industrial preparation.
The present inventors have found that it is possible to overcome the abovementioned drawbacks, by combining incompactable fillers and/or low-density fillers with a binder fatty phase having a specific composition.
In one aspect, the present disclosure provides cosmetic compositions in compact powder form for making up and/or caring for the skin, such as the face, comprising a pulverulent phase and a fatty phase comprising at least one solid fatty phase, wherein:
In another aspect, the present disclosure provides cosmetic compositions in compact powder form for making up and/or caring for the skin, such as the face, comprising:
In another aspect, the present disclosure provides cosmetic compositions in compact powder form for making up and/or caring for the skin, such as the face, comprising:
In yet another aspect, the present disclosure provides cosmetic compositions in compact powder form for making up and/or caring for the skin, such as the face, comprising:
In still another aspect, the present disclosure provides cosmetic compositions in compact powder form for making up and/or caring for the skin, such as the face, comprising:
According to some embodiments, the compositions disclosed herein do not comprise 10% by weight of carnauba wax, 6% by weight of magnesium stearate and 5% by weight of amorphous magnesium and/or aluminium silicate, relative to the total weight of the composition.
In another aspect, the present disclosure provides the use of either a pulverulent phase as described above, or of at least one filler chosen from incompactable fillers and low density fillers in an amount of greater than or equal to 5% by weight relative to the total weight of the composition, in combination with a fatty phase comprising at least one solid fatty phase, for example, as described above for the preparation of a compact powder cosmetic compositions with satisfactory cohesion and erosion properties.
According to still another aspect, the present disclosure provides processes for making up and/or caring for the skin, comprising applying to the skin at least one composition decribed herein.
The compositions disclosed herein can have satisfactory cohesion and erosion properties, i.e., satisfactory stability on storage and do not change or undergo little change when subjected to impacts. The compositions also have a good capacity for take-up and application.
Cohesion and Erosion Measurements
Cohesion and erosion may be measured according to the protocols described below.
The pulverulent phase requires preformulation with a binder known as a reference liquid binder. The composition of the reference liquid binder, which is also given in Example 1 below, is as follows:
The mixture of preserving agents Phenonip® contains (weight %):
The mixture of reference liquid binder (8.8% by weight) and of the pulverulent phase (91.2% by weight) is placed in a 57×39×05 mm rectangular aluminium crucible.
The mixture (10.5 g) is poured into the crucible and a pressure of 2×107 Pa (200 bar) is then applied.
It is estimated that the product is not eroded homogeneously when, once the surface of the product, which is compact in the crucible, is rubbed with the fingers or with a dry sponge, for example a rectangular sponge such as the sponge sold under the name Yukilon Standard® by the company Yukigaya, it crumbles, comes away in lumps and/or wears away by hollowing. The erosion of the product is then considered as being irregular and non-homogeneous over the entire surface.
The drop test protocol consists of subjecting the compact, which is in a proportion of 10.5 g in a crucible as defined above, to 10 standardized drops over a height of 20 cm onto a sandstone floor tile 30 mm thick; the base of the dish is oriented towards the receiving surface of the sandstone floor tile. The loss of mass of product is then measured, after which the percentage loss of mass of powder is determined.
When the compositions have good cohesion properties, they may have a loss of mass in the drop test of less than 12% by weight, for example, less than 10% by weight, or even less than 8% by weight.
As previously specified, the compositions are provided in the form of compact powders. This compacted feature is obtained by subjecting to a compression the mixture of the particulate phase and the associated fatty binder.
The compositions in the form of a compact powder may be prepared by mixing the whole components of the particulate phase (fillers and pigments) and then adding under agitation to this mixture the components constituting the fatty phase. The mixture is then ground, sieved, and then poured into an assay crucible and compacted. This compacting is generally realized using a press applying a pressure from 50 to 250 bars to obtain the compact powder.
Consequently, the compositions are different from the termed poured particulate compositions, which are just prepared by mixing a fatty phase in the molded state with a particulate phase.
Since the compositions of the present disclosure are provided in the form of a compact powder, they have a better chance, compared to poured-type compositions, of being disintegrated in the form of “free” solid particles.
Thus, one can, after the unpacking of a compact composition as presently disclosed, recuperate its particulate phase, which is not possible with poured compositions.
The unpacking can be done according to the following process: the compacted product is broken using a spatula over a sieve (250 p) and then the obtained heaps of powder are sieved. Thus, the particulate phase of the compact powder is recovered in the form of “free” solid particles.
Pulverulent Phase
The term “pulverulent phase,” as used herein, includes any solid compound and mixture of solid compounds whose melting point is higher than 250° C. and may even be much higher.
The pulverulent phase generally comprises at least one filler and/or at least one pulverulent dyestuff.
The at least one filler may be chosen from incompactable fillers, low-density fillers, additional fillers, and mixtures thereof.
The term “additional filler,” as used herein, means any filler other than the incompactable fillers and/or the low-density fillers described herein.
The at least one pulverulent dyestuff may be chosen from pigments and nacres usually used in cosmetic and/or dermatological compositions.
In some embodiments, the at least one filler is chosen from hydrophobic- treated and hydrophobic-coated powders.
The term “hydrophobic-treated and hydrophobic-coated powders,” as used herein, means any powder surface-treated with a hydrophobic agent, for example, as described below.
The hydrophobic agent may be chosen from, for example, silicones, including methicones, dimethicones, and perfluoroalkylsilanes; fatty acids, for example stearic acid; metal soaps, for example aluminium dimyristate, the aluminium salt of hydrogenated tallow glutamate, perfluoroalkyl phosphates, perfluoroalkylsilanes, perfluoroalkylsilazanes, polyhexafluoropropylene oxides, polyorganosiloxanes comprising perfluoroalkyl perfluoropolyether groups, amino acids; N-acylamino acids or salts thereof; lecithin, isopropyl triisostearyl titanate, and mixtures thereof.
The N-acylamino acids may comprise an acyl group having from 8 to 22 carbon atoms, for example a 2-ethylhexanoyl, caproyl, lauroyl, myristoyl, palmitoyl, stearoyl, or cocoyl group. The salts of these compounds may be, for example, the aluminium, magnesium, calcium, zirconium, zinc, sodium, or potassium salts. The amino acid may be, for example, lysine, glutamic acid or alanine.
The term “alkyl” as used above, denotes an alkyl group having from 1 to 30 carbon atoms, for example, from 5 to 16 carbon atoms.
Pigments and hydrophobic-treated fillers are described, for instance, in patent application EP 1,086,683 A.
The pulverulent phase of the compositions may comprise a hydrophobic- treated powder or mixture of powders in an amount of greater than or equal to 50% by weight, for example, greater than or equal to 60% by weight, or even greater than or equal to 70% by weight, relative to the total weight of the pulverulent phase.
As described above, the compositions disclosed herein may comprise at least one incompactable filler and/or at least one low-density filler.
Incompactable Fillers
In some embodiments, the compositions comprise at least one incompactable filler in an amount of greater than or equal to 5% by weight, relative to the total weight of the composition.
The term “incompactable filler,” as used herein, means a powder which, at and above a certain amount that will depend on the material under consideration, for example, from an amount of greater than or equal to 5% by weight relative to the total weight of the composition, does not have good compactability using a manual press, for example, under a pressure of 2×107 Pa (200 bar) and/or is detrimental to the production of products with good impact strength, for example, having a loss of mass of greater than 12% in the drop test, and/or that does not make it possible to obtain a compact product that can be eroded homogeneously.
The at least one incompactable filler may be organic or mineral, and in spherical or lamellar form.
Incompactable spherical fillers that may be used include:
Low-Density Fillers
In other embodiments, the compositions comprise at least one low-density filler in an amount of at least 5% by weight relative to the total weight of the composition.
The term “low-density filler,” as used herein, means a filler whose untamped density, measured via the protocol given below, ranges from 0.01 to 0.50 g/cm3, for example, ranging from 0.05 to 0.50 g/cm3 or from 0.10 to 0.50 g/cm3.
Protocol for Measuring Untamped Density (DUT):
A volume of from 240 to 250 ml of powder is poured into a 250 ml measuring cylinder having a mass M0 (g), using a funnel. The volume V0 (cm3) of powder poured in is then read on the cylinder and the cylinder filled with powder is weighed to measure the mass M1 (g).
The untamped density is determined according to the following formula:
DUT=(M1−M0)/V0
The low-density fillers may also be characterized by a tamped density, measured via the protocol given below, ranging from 0.01 to 0.80 g/cm3, for example, ranging from 0.05 to 0.80 g/cm3 or from 0.10 to 0.80 g/cm3.
Protocol for Measuring Tamped Density (DT):
A volume of from 240 to 250 ml of powder is poured into a 250 ml measuring cylinder having a mass M0 (g) using a funnel. The volume V0 (cm3) of powder poured in is then read on the cylinder and the cylinder filled with powder is weighed to measure the mass M1 (g).
The cylinder is then placed on the STAV 2003@ machine from Stampf Volumeter. The cylinder is then subjected to a series of 2500 tamping blows, and the volume Vn (volume after the nth series of 2500 tamping blows) of the powder in the cylinder is then measured at the end of each series.
Once Vn−Vn+1≦(2×Vn)/100, the tamping of the cylinder is stopped and the volume Vn (cm3) is noted.
The tamped density is determined according to the following relationship:
DT=(M1−M0)/Vn
The low-density fillers useful herein may be chosen from the list of incompactable fillers given above as well as from the fillers described in the following table:
The composition according to the present disclosure may comprise at least one incompactable filler or a mixture of at least one incompactable filler and/or at least one low-density filler in an amount ranging from 5% to 15% by weight, for example from 5% to 13% or 5% to 10% by weight relative to the total weight of the composition.
The pulverulent phase may also further comprise at least one additional filler. These fillers may be mineral or organic and of any shape, such as platelet-shaped, spherical or oblong, irrespective of their crystallographic form (for example lamellar, cubic, hexagonal, orthorhombic, etc.). Additional fillers that may be used in the compositions include talc, mica, silica, kaolin, polyamide (Nylon®) powder, poly-β-alanine powder, polyethylene powder, tetrafluoroethylene polymer (Teflon®) powders, lauroyllysine, starch, boron nitride, acrylic acid polymer powders, silicone resin microbeads (for example Tospearls® from Toshiba), precipitated calcium carbonate, magnesium carbonate, magnesium hydrocarbonate, hydroxyapatite, hollow silica microspheres, and glass or ceramic microcapsules.
The additional filler or mixture of additional fillers may be present in an amount ranging from 40% to 95% by weight, for example, from 45% to 85% or 45% to 70% by weight relative to the total weight of the composition.
As mentioned above, the compositions according to the present disclosure may also comprise at least one pulverulent dyestuff chosen from pigments and nacres.
The pigments may be white or colored, mineral and/or organic, and coated or uncoated. Mineral pigments that may be used herein include titanium dioxide, optionally surface-treated, zirconium oxide or cerium oxide, and also iron oxide or chromium oxide, manganese violet, ultramarine blue, chromium hydrate and ferric blue. Organic pigments that may be used include carbon black, pigments of D & C type and lakes based on cochineal carmine or on barium, strontium, calcium or aluminium.
The nacres may be chosen from white nacreous pigments such as mica coated with titanium or with bismuth oxychloride, colored nacreous pigments such as titanium mica with iron oxides, titanium mica with, for example, ferric blue or chromium oxide, titanium mica with an organic pigment of the abovementioned type and nacreous pigments based on bismuth oxychloride.
The pulverulent dyestuff may be present in the compositions in an amount ranging from 0.5% to 30% by weight, for example from 1% to 22% or 3% to 18% by weight relative to the total weight of the composition.
Fatty Phase:
As mentioned above, the fatty phase may also be referred to as a “binder” and serves as a dispersing medium for the particulate phase. The fatty phase may be present in the presently disclosed compositions in an amount ranging from 12% to 35% by weight, for example, from 15% to 30% by weight relative to the total weight of the composition.
Solid Fatty Phase:
The compositions as disclosed herein comprise at least one fatty phase comprising at least one solid fatty phase, also known as a “solid binder” in an amount such that the weight ratio of the at least one solid fatty phase to the at least one incompactable filler and/or at least one low-density filler is greater than or equal to 1, such as greater than or equal to 1.5.
As used herein, the term “solid binder” is understood to mean a fatty phase whose melting point may be greater than or equal to 30° C., for instance ranging from 30° C. to 250° C., such as from 30° C. to 230° C.
The at least one solid fatty phase may comprise at least one compound chosen from waxes and metal soaps, and mixtures thereof.
As used herein, the term “wax” is understood to mean a lipophilic fatty compound, which is solid at room temperature and atmospheric pressure (760 mmHg, i.e. 105 Pa), which undergoes a reversible solid/liquid change of state, and which for instance has a melting point of greater than or equal to 30° C., for example, greater than or equal to 55° C., such as up to 120° C., which may be up to 250° C., such as up to 230° C.
By bringing the wax to its melting point, it is possible to make it miscible with the oils and to form a microscopically homogeneous mixture, but upon returning the temperature of the mixture to room temperature, the recrystallization of the wax in the oils of the mixture is obtained.
According to the present disclosure, the melting point values correspond to the melting peak measured using a differential scanning calorimeter (DSC), for example the calorimeter sold under the name DSC 30 by the company Mettler, with a temperature rise of 5 or 10° C. per minute.
For the purposes of the present disclosure, the waxes may be those generally used in cosmetics or dermatology. They may be, for example, hydrocarbon-based waxes, silicone waxes and/or fluoro waxes, optionally comprising ester or hydroxyl functional groups. They may also be of natural or synthetic origin.
Non-limiting illustrations of the waxes that may be used may be made of:
According to one embodiment of the present disclosure, the at least one solid fatty phase may comprise at least one wax chosen from carnauba waxes and paraffin waxes, and mixtures thereof.
According to another embodiment of the present disclosure, the at least one solid fatty phase may comprise at least one wax that is totally or partially in powder form, such as in micronized form, to facilitate its use in the preparation of the cosmetic composition.
Among the waxes that may be used in powder form, non-limiting mention may be made of, for example, the carnauba wax microbeads sold under the name Microcare 350® by the company Micro Powders and the paraffin wax microbeads sold under the name Microease 114S® by the company Micro Powders.
The solid binder may also be chosen from metal soaps.
Among these soaps, non-limiting mention may be made of, for example, the metal soaps of fatty acids comprising from 12 to 22 carbon atoms, such as those comprising from 12 to 18 carbon atoms.
In one embodiment of the present disclosure, the metal of the metal soap may be chosen from zinc and magnesium.
The fatty acid may be chosen from, for example, lauric acid, myristic acid, stearic acid and palmitic acid.
Non-limiting examples of metal soaps that may be used include zinc laurate, magnesium stearate, magnesium myristate and zinc stearate, and mixtures thereof.
According to one aspect of the present disclosure, the at least one solid fatty phase may comprise at least one metal soap that is totally or partially present in powder form.
The at least one solid fatty phase may be present in an amount greater than or equal to 35% by weight, for instance greater than or equal to 40% by weight, such as greater than or equal to 50% by weight, relative to the total weight of the fatty phase.
The weight ratio of the at least one solid fatty phase to the at least one incompactable filler or at least one low-density filler can range, for example, from 1 to 4, for instance, from 1 to 3, such as from 1 to 2.5.
The composition as disclosed herein can comprise the at least one solid fatty phase, for example, in an amount ranging from 8% to 25% by weight, such as from 10% to 22% by weight, and from 10% to 20% by weight relative to the total weight of the composition.
Liquid Fatty Phase:
The fatty phase of the composition according to the present disclosure may also comprise a liquid fatty phase comprising at least one oil. This oil may be chosen from the oils conventionally used as binders in compact powders.
Non-limiting examples of the oils that may be used include:
Among the compounds of formula (I) that may be used as disclosed herein, non-limiting mention may be made of, for example, the products sold under the names X22-819®, X22-820®, X22-821® and X22-822® by the company Shin-Etsu.
The composition according to the present disclosure may also comprise a liquid fatty phase in an amount ranging from 4% to 15% by weight, for instance, from 6% to 13% by weight, such as from 7% to 13% by weight, relative to the total weight of the composition.
According to one aspect of the present disclosure, the liquid fatty phase and the at least one incompactable filler or at least one low-density filler are present in the compositions as disclosed herein such that the weight ratio of the liquid fatty phase to the at least one incompactable filler or at least one low-density filler is less than or equal to 3, such as than or equal to 2.5, for instance less than or equal to 2 or even less than or equal to 1.5.
According to one embodiment of the present disclosure, the composition is free of liquid fatty phase.
Needless to say, a person skilled in the art will take care to adjust the amounts of the at least one solid fatty phase and possibly the liquid phase of the composition according to the present disclosure such that the expected properties in terms of cohesion and matting effect over time are satisfactory.
Additives:
The composition may also comprise at least one adjuvant often used in cosmetics, such as water-soluble or liposoluble coloring agents, preserving agents, cosmetic active agents, moisturizers, UV-screening agents, thickeners, water, surfactants and/or fragrances.
Needless to say, a person skilled in the art will take care to select the optional at least one adjuvant added to the compositions such that the beneficial properties intrinsically associated with the compositions are not, or are not substantially, adversely affected by the envisaged addition.
The compositions as disclosed herein can be in the form of a makeup product of compact powder type, such as a makeup rouge, an eyeshadow, a face powder, a foundation, a concealer product or a body makeup product, or alternatively in the form of a facial care product or a body care product.
The invention is illustrated in greater detail by the non-limiting examples described below. Other than in the examples, or where otherwise indicated, all numbers expressing quantities of ingredients, reaction conditions, and so forth used in the specification and claims are to be understood as being modified in all instances by the term “about.” Accordingly, unless indicated to the contrary, the numerical parameters set forth in the following specification and attached claims are approximations that may vary depending upon the desired properties sought to be obtained herein. At the very least, and not as an attempt to limit the application of the doctrine of equivalents to the scope of the claims, each numerical parameter should be construed in light of the number of significant digits and ordinary rounding approaches.
Notwithstanding that the numerical ranges and parameters setting forth the broad scope are approximations, the numerical values set forth in the specific example are reported as precisely as possible. Any numerical value, however, inherently contains certain errors necessarily resulting from the standard deviation found in its respective testing measurements.
The mixture of preserving agents Phenonip® contains:
(a) Composition: According to the Invention
The composition was prepared by mixing together the mixture of powders and then adding the fatty phase thereto, this mixture was then ground and screened until a homogeneous mixture was obtained. Some of the composition (10.5 g) was placed in a dish and then compacted at a pressure of 2×107 Pa (200 bar).
The composition had a cohesion such that the loss of product during the drop test was 2% by weight.
Application of the compact powder to the face afforded a makeup result that showed good color homogeneity and good matting throughout the day.
91.2% by weight of the same pulverulent phase was formulated in the presence of 8.8% by weight of a liquid binder, i.e., 3.60 g of 2-ethylhexyl 4-p-methoxycinnamate, 2.20 g of polydimethylsiloxane and 2.20 g of isocetyl stearate and 0.80 g of a mixture of preserving agents:
The compacted composition was tested to evaluate its mechanical properties. The loss of product during the drop test was 17.6% by weight, which reflects a cohesion defect. In addition, the erosion of the compacted product with a dry sponge was found to be too great, since the product crumbled away upon contact with the sponge and the compact wore away by hollowing. The liquid binder therefore did not make it possible to obtain a satisfactory compact powder.
(a) Composition According to the Invention
The composition was prepared by mixing together the mixture of powders (iron oxides, talc, silica and carnauba wax) and then adding the oils (hydrogenated polydecene and fluorosilicone) thereto, and this mixture was then ground and screened until a homogeneous mixture was obtained. Some of the composition (10.5 g) was placed in a dish and then compacted at a pressure of 2×107 Pa (200 bar).
The compacted composition had a cohesion such that the loss of product during the drop test was less than 5.72% by weight.
The compact powder obtained afforded a makeup result that showed good matting throughout the day when applied to the face.
(b) Comparative Composition 91.2% by weight of the same pulverulent phase was formulated in the presence of 8.8% by weight of a liquid binder, i.e., 3.60 g of 2-ethylhexyl 4-p-methoxycinnamate, 2.20 g of polydimethylsiloxane and 2.20 g of isocetyl stearate, and 0.80 g of a mixture of preserving agents:
The composition was prepared in the same manner as described in (a).
The compacted composition had a cohesion such that the loss of product during the drop test was greater than 12% by weight. The erosion of the compacted product was too great. The product crumbled away on contact with a dry sponge and the compact was worn away by hollowing. The liquid binder therefore did not make it possible to obtain a compact powder that was satisfactory in terms of cohesion and erosion.
(a) Composition According to the Invention:
The composition was prepared by mixing together the mixture of powders (iron oxides, silica, polyurethane, etc.) and then adding the oils (isononyl isononanoate, fluorosilicone and 2-ethylhexyl 4-p-methoxycinnamate) thereto, and this mixture was then ground and screened until a homogeneous mixture was obtained. Some of this composition (10.5 g) was placed in a dish and then compacted at a pressure of 2×107 Pa (200 bar).
The compacted composition had a cohesion such that the loss of product during the drop test was 2.2% by weight.
The compact powder foundation obtained afforded a makeup result that showed good matting throughout the day when applied to the face.
91.2% by weight of the same pulverulent phase was formulated in the presence of 8.8% by weight of a liquid binder, i.e. 3.60 g of 2-ethylhexyl 4-p-methoxycinnamate, 2.20 g of polydimethyl siloxane and 2.20 g of isocetyl stearate and 0.80 g of a mixture of preserving agents:
The compacted composition had a cohesion such that the loss of product during the drop test was 2.38% by weight.
However, the erosion of the compacted product was too great, the product crumbles away on contact with the sponge and the compact becomes worn away by hollowing. The liquid binder therefore did not make it possible to obtain a compact powder that shows satisfactory erosion.
Although the present disclosure has been described with reference to particular embodiments, it is to be understood that these embodiments are merely illustrative of the principles and applications of the present disclosure. It is therefore to be understood that numerous modifications may be made to the illustrative embodiments and that other arrangements may be devised without departing from the spirit and scope of the present present disclosure as defined by the appended claims.
| Number | Date | Country | Kind |
|---|---|---|---|
| 04 50148 | Jan 2004 | FR | national |
This non-provisional application claims the benefit of French Application No. 04/50148, filed Jan. 27, 2004, and U.S. Provisional Application No. 60/541,366, filed Feb. 4, 2004, both hereby incorporated by reference.
| Number | Date | Country | |
|---|---|---|---|
| 60541366 | Feb 2004 | US |
