PIGMENT COMPRISING RAPHANUS SATIVUS EXTRACT AND MONTMORILLONITE

Abstract

A pigment for cosmetic applications is provided, which exhibits excellent color and stability characteristics, while being fully plant-based, edible and of natural origin.

Claims

1. A pigment for cosmetic applications, comprising micronized Raphanus sativus L. root extract and montmorillonite clay.

2. The pigment according to claim 1, comprising micronized Raphanus raphanistrum subsp. sativus (L.) Domin root extract.

3. The pigment according to claim 1, wherein the micronized Raphanus sativus L. root extract has a median particle size (D50) of from about 1.0 μm to about 7.5 μm.

4. The pigment according to claim 1, wherein the micronized Raphanus sativus L. root extract has a particle size 90% percentile (D90) of from about 4.0 μm to about 16.0 μm.

5. The pigment according to claim 1, wherein the weight ratio of micronized Raphanus sativus L. root extract to montmorillonite clay is from about 1:2 to about 2:1.

6. The pigment according to claim 1, wherein the pigment has a red, pink, purple, blue or green color.

7. The pigment according to claim 1, claims 1 to 6, wherein the pH of the pigment is from about 2.0 to about 4.0.

8. The pigment according to claim 1, wherein the pH of the pigment is from about 7.2 to about 8.0.

9. The pigment according to claim 1, further comprising an acid.

10. The pigment according to claim 1, further comprising a base.

11. The pigment according to claim 1, further comprising a polysaccharide.

12. The pigment according to claim 1, comprising from about 10 wt % to about 40 wt % of micronized Raphanus sativus L. root extract, from about 20 wt % to about 50 wt % of montmorillonite clay, from about 2 wt % to about 15 wt % of citric acid, and from about 10 wt % to about 40 wt % of maltodextrin.

13. The pigment according to claim 1, wherein at least all solid components of the pigment are micronized.

14. A cosmetic composition comprising the pigment according to claim 1 and a cosmetically acceptable excipient.

15. The cosmetic composition according to claim 14, which is a make-up, and in particular a lipstick composition.

16. The pigment according to claim 12, comprising from about 20 wt % to about 30 wt % of micronized Raphanus sativus L. root extract, from about 30 wt % to about 40 wt % of montmorillonite clay, from about 5 wt % to about 10 wt % of citric acid, and from about 20 wt % to about 30 wt % of maltodextrin.

17. The pigment of claim 9 which comprises citric acid.

18. The pigment of claim 10 which comprises a basic salt.

19. The pigment of claim 11 which comprises maltodextrin.

20. The pigment of claim 15 which is a lipstick composition.

Description

Example 1: Raphanus sativus L. Root Extract

[0083] Raphanus sativus L. root extract is commercially available from several suppliers.

[0084] For the present studies, “Deodorized Red Radish Extract (Powder)” was obtained from Yunnan Rainbow Bio-tech. Corp., Ltd. This extract is obtained from red radish of the species Raphanus raphanistrum subsp. sativus (L.) Domin.

[0085] According to the supplier, this commercial extract has the following composition: 42% red radish extract, 42% maltodextrin, 8% citric acid, and 8% water. It is prepared as follows: [0086] extraction with water [0087] filtration [0088] adsorption and desorption with ethanol (70%) [0089] deodorization [0090] concentration [0091] addition of maltodextrin [0092] addition of citric acid and/or KOH to adjust the pH [0093] homogeneization [0094] spray drying [0095] micronization

[0096] The commercial extract is in the form of a red powder.

[0097] For the present studies, two different batches of “Deodorized Red Radish Extract (Powder)” from Yunnan Rainbow were used: LT160901 and LT151102.

[0098] The anthocyanin content of the two batches was analyzed by HPLC-UV at 520 nm after separation on a C.sub.18 column, using perlagonidin-3-O-glucoside as an external standard and applying a molecular weight correction factor (MWCF) after identification of the main compounds with LC-TOF-MS (mainly perlargonidin and anthocyanidin moiety). It was found that LT160901 had an anthocyanin content of 28.72%, and LT151102 of 30.89%.

Example 2: Red Pigment Preparation

[0099] The Raphanus sativus L. root extract of example 1 was mixed with montmorillonite clay in a weight ratio of 5:3 in the presence of water. For instance, for a batch of 250 kg of red pigment, 150 kg of water, 60.3 kg of “Deodorized Red Radish Extract (Powder)” and 36.4 kg of montmorillonite clay (“argile blanche-rosée”, ref: CosWHITE™, supplied by Argile du Velay, France) were mixed and stirred at room temperature until homogenous. The pH was adjusted to about 2.8 by addition of 3.9 kg of citric acid.

[0100] The thus obtained mixture was homogenized by stirring at room temperature and then subjected to spray drying (on a GEA Niro spray dryer) and air jet micronization. Alternatively, it would also be possible to use oven drying, without any influence on the resulting product.

[0101] For one particular sample, the particle size distribution was measured before and after the micronization: before micronization D10=3.89 μm, D50=19.71 μm, D90=53.68 μm; after micronization: D10=0.66 μm, D50=1.91 μm, D90=4.19 μm.

[0102] The red pigment used for the studies described below was prepared according to the above process and had the following composition:

TABLE-US-00001 Raw Concen- Material Origin INCI tration Raphanus Botanical: Raphanus sativus Antho- 20-30 wt % sativus L. L. cyanins root extract Maltodextrin Botanical: Zea Mays L. or Malto- 20-30 wt % Manihot esculenta Crant dextrin Montomoril- Mineral Montomoril- 30-40 wt % lonite clay lonite Citric acid Botanical: Zea Mays L. or Citric acid  5-10 wt % Manihot esculenta Crantz

[0103] Therefore, the red pigment of the present invention is of 100% natural origin content and 55-70% of natural content according the ISO 16128 assessment.

Example 3: Characteristics of Red Pigment

[0104] The red pigment of example 2 is a red powder. It has a mean particle size (D50) of about 2 μm to about 5 μm.

[0105] The anthocyanin content, as determined by HPLC, was from about 12 wt % to about 18 wt %.

[0106] The red pigment has a pH of about 2.5 to about 3.5 at 1% in distilled water.

[0107] Analysis of the powder by LC-TOF-MS in positive ion mode revealed at least 30 different anthocyanins mainly based on perlargonidin (22), delphinidin (2), cyanidin (5) and malvinidin (1) cores.

[0108] Colorimetric analysis provided the following results (E1% is the absorbance at the given wavelength for 1 g of product in 100 ml of solvent):

TABLE-US-00002 L* a* b* C* h E1% at 520 nm, pH 3 48.9 38.5 17.5 42.3 24.4 27.9

[0109] Thus, the color of the red pigment of the present invention corresponds to Pantone 1805 C.

Example 4: Stability Studies

[0110] Stability at Room Temperature

[0111] The stability of a first batch of the red pigment of example 3 was tested at room temperature, protected from light and moisture. The results were as follows:

TABLE-US-00003 Microbiological Total Yeasts Plate and Color Dry Count Moulds L* a* b* DE2000 matter [cfu/g] [cfu/g] T0 49.7 38.0 17.7 — 95.4 <100 <100 wt % 1 month 49.1 36.9 16.7 0.85 95.2 <100 <100 wt % 2 months 50.7 38.6 17.7 1.00 96.2 <100 <100 wt % 3 months 50.6 38.4 17.3 0.91 95.8 <100 <100 wt % 4 months 48.9 37.3 16.9 0.87 96.1 <100 <100 wt % 9 months 49.4 36.7 15.8 1.09 94.4 <100 <100 wt % 12 months 48.6 36.5 15.8 1.52 97.1 <100 <100 wt % 18 months 49.3 38.4 16.9 0.95 93.3 <100 <100 wt %

[0112] Thus, the red pigment of the present invention is perfectly stable and complies with the microbiological requirements (Total Plate Count=TPC; Yeasts and Mould=Y & M) for cosmetic ingredients even after 9 months.

[0113] Heat Stability

[0114] The stability of the first batch of the red pigment of example 3 was also tested at increased temperature:

TABLE-US-00004 Microbiological Color TPC Y & M L* a* b* DE2000 [cfu/g] [cfu/g] rt 51.6 39.2 18.5 — 191 0 30 min at 105° C. 50.1 36.0 16.5 2.02 55 0 30 min at 110° C. 48.5 34.2 15.2 3.84 0 0 30 min at 120° C. 49.3 35.5 16.3 2.78 27 0

[0115] As can be seen from the above, the red pigment of the present invention exhibits good stability even at high temperature. This allows for thermal debacterization if necessary:

TABLE-US-00005 Microbiological Color TPC Y & M L* a* b* DE2000 [cfu/g] [cfu/g] rt 51.6 39.2 18.5 — 191 0 30 min at 120° C. 43.8 34.1 14.8 2.32 0 0 60 min at 120° C. 50.6 37.4 16.7 1.04 0 0 90 min at 120° C. 49.7 35.6 15.6 1.28 0 0

[0116] Suntest

[0117] The color stability of a second batch of the red pigment of example 3 was tested at 450 W/m.sup.2:

TABLE-US-00006 L* a* b* C* h DE2000 T0 48.3 36.3 15.7 39.6 23.4 — 7 h at 450 W/m.sup.2 48.4 36.6 16.1 40.4 23.7 0.25 8 h at 450 W/m.sup.2 49.4 38.0 16.9 41.6 24 1.33 12 h at 450 W/m.sup.2  49.6 37.2 16.2 40.6 23.6 1.38

[0118] Again, the red pigment of the present invention was found to have a good stability.

Example 5: Impact of Micronization and Montmorillonite Clay

[0119] In order to determine the impact of micronization and/or montmorillonite clay, a set of comparative tests was run in a lipstick base containing 10 wt % of red pigment powder.

[0120] The following lipstick base was used:

TABLE-US-00007 Phase Ingredient Concentration A Butyrospermum parkii butter 37.5 wt % A Cera alba 37.5 wt % A Caprylic/capric triglycerides 7.5 wt % B Castor oil 17.5 wt % B Red pigment 10 wt %

[0121] The following four red pigment powders were tested: [0122] Comparative sample A: commercial Raphanus sativus L. root extract from Yunnan Rainbow as described in example 1 [0123] Comparative sample B: same as comparative sample A, but micronized [0124] Comparative sample C: red pigment of example 2, but without micronization [0125] Red pigment of the present invention: red pigment of example 2

[0126] Phase A was prepared by blending butyrospermum parkii butter, cera alba and caprylic/capric triglycerides at a temperature of 70° C. until homogeneous. To obtain phase B, a mixture of the respective red pigment powder and the castor oil was homogenized in a turrax blender for 2 min at room temperature. The two phases were combined at 75° C. and blended in the turrax blender for 2 min. The thus obtained lipstick composition was cooled down to room temperature unde magnetic agitation. Finally, it was crushed between glass slabs and applied to a contrast card using a film applicator (film thickness: 50 μm).

[0127] L,a,b measurements were performed on a Spectrocolorimeter Konica-Minolta 3600d (D65, L*,a*,b*,h,C*,Y) and DeltaE(00) was measured to see the color and opacity differences between the different red pigments in lipstick base. The opacity is a measure of covering power, with 100% opacity meaning full coverage. The opacity is calculated as CR (%)=((Y black*100)/Y white)

[0128] The results are shown in the following table:

TABLE-US-00008 CR/ opacity Micron- Montmoril- Hue Chroma (cover- ization lonite (h) (C*) age) Comparative sample A no no 26.0 35.3 13.3% Comparative sample B yes no 24.3 52.0 35.6% Comparative sample C no yes 15.9 15.8 42.3% Red pigment of the yes yes 29.5 60.4 30.2% present invention

[0129] As can be seen from the above, micronization leads to an increase in chroma and coverage, while the addition of montmorillonite clay improves the coverage, but decreases chroma and hue.

[0130] Best results were observed for the red pigment of the present invention, involving both micronization and montmorillonite clay, which showed a strong increase in chroma, and clear increases for both hue and coverage.

Example 6: Anti-Oxidant Activity (in vitro)

[0131] The anti-oxidant properties of Raphanus sativus L. root extract was evaluated using human normal keratinocytes (NHEKs) by quantification of Reactive Oxygen Species (ROS) production after oxidative stress exposure according to the dichlorodihydrofluorescein diacetate (DCFH-DA; “Dichloro-dihydro-fluorescein diacetate (DCFH-DA) assay: a quantitative method for oxidative stress assessment of nanoparticle-treated cells”. Aranda et al. Toxicol In Vitro. 2013, 27(2):954-63.) method. In contact with cells, DCFH-DA is cleaved inside the cell to DCFH which is able to interact with reactive oxygen species (ROS) during oxidative stress leading to fluorescence emission. Consequently, the fluorescence emitted is correlated to the antioxidant property of the tested compound.

[0132] Cell Culture and Pre-Treatment

[0133] The cell culture was done on primary cells freshly isolated from biopsies.

[0134] Normal Human Epidermal Keratinocytes (NHEKs) were seeded in a black plate with a glass bottom at 20′000 cells per well in 96-wells plates with a type I collagen pre-coating in quadruplicate. The cells were incubated for 24 hours in complete medium (Epilife medium supplemented with HKGS) at 37° C. with 5% CO.sub.2.

[0135] After 24 hours of culture, the cells were treated with Resveratrol (comparative example) or different concentrations of the commercial Raphanus sativus L. root extract of example 1 in complete medium, or with just complete medium (control).

[0136] Cells were then incubated for another 24 hours at 37° C., 5% CO.sub.2.

[0137] ROS measurement

[0138] After 24 h of incubation, 2′,7′-dichlorofluorescin diacetate (DCFH-DA) probe was added to the wells at 50 μM for at least 30-45 minutes at 37° C.

[0139] Cells were then washed two times with PBS buffer and treated with tert-butyl hydroperoxide solution (TBP) at 5 mM in PBS buffer to cause oxidative stress. For comparison, untreated cells were left in PBS buffer.

[0140] Finally, the emitted fluorescence was measured in darkness by excitation wavelength at 488 nm and emission wavelength at 525 nm with microplate reader (TECAN).

[0141] The study was carried out in duplicate and with n=4.

[0142] Statistical Analysis

[0143] A Shapiro-Wilk normality test was performed to evaluate whether the data follows the Gaussian Law. The results did not follow the Gaussian Law.

[0144] As a consequence, a non-parametric statistical analysis was performed by Kruskal-Wallis ANOVA followed by Mann Whitney U test.

[0145] Results

[0146] The results are summarized in the following table:

TABLE-US-00009 Compari- Mean son to relative Standard oxidative to TBP Deviation stress, no condition (SD) active No oxidative stress (no TBP, no 22.4% 6.32% active) Oxidative No active  100% 12.65% — stress 200 μM Resveratrol 24.0% 6.55% −76%*** (5 mM 0.1% (w/v) Raphanus 23.4% 23.28% −77%*** TBP) sativus L. root extract 1.0% (w/v) Raphanus 15.8% 6.04% −84%*** sativus L. root extract ***p < 0.001

[0147] It was confirmed that TBP, which was used to induce oxidative stress, significantly increased the amount of reactive oxygen species (ROS) compared to the untreated control (p<0.001).

[0148] Treatment with Resveratrol at 200 μM was used as a positive control.

[0149] Under the same conditions, Raphanus sativus L. root extract was found to significantly reduce ROS production in a dose-dependent manner.

Example 7: Dispersion in Different Solvents

[0150] The dispersion of the red pigment of example 2 at a concentration of 10 wt % was tested in the following solvents: [0151] Tris(2-octyldodecyl) citrate (PELEMOL® TGC) [0152] Triisostearyl citrate (PELEMOL® TISC) [0153] Refined castor oil (Radia 6132) [0154] Polyglyceryl-3 diisostearate [0155] Dodecane (Parafol® 12-97) [0156] Jojoba seed oil [0157] Caprylic/capric triglyceride [0158] Propanediol dicaprylate (DUB ZENOAT®) [0159] Isononyl isononanoate (DUB ININ 14031) [0160] Octyldodecanol (EUTANOL G) [0161] Isocetyl stearoyl stearate (DUB SSIC) [0162] Sunflower seed oil

[0163] To assess dispersion, microscope images were taken with 10×zoom without polarized light.

[0164] It was found that the red pigment was well dispersed in refined castor oil, tris(2-octyldodecyl) citrate, triisostearyl citrate, and polyglyceryl-3 diisostearate. Of these four, only tris(2-octyldodecyl) citrate is fluid, while the other three solvents are viscous. Furthermore, polyglyceryl-3 diisostearate was found to amend the color of the pigment, making it more blueish. The use of refined castor oil is particularly advantageous because it is fully natural.

[0165] The use of dodecane, jojoba seed oil, caprylic/capric triglyceride, propanediol dicaprylate, isononyl isononanoate, octyldodecanol, and sunflower seed oil led to a poor dispersion with agglomerates. Dispersion was slightly better for isocetyl stearoyl stearate.

Example 8: Impact of Micronization in Lipstick Formulation

[0166] A first lipstick base formulation was prepared as described in example 5.

[0167] The thus obtained lipstick formulations were applied manually on black-and-white contrast cards; and the spreadability, hue, chroma and opacity were measured using a spectrocolorimeter Konica-Minolta 3600d.

[0168] The results were as follows:

TABLE-US-00010 CR/ Hue Chroma opacity Spreadability (h) (C*) (coverage) Lipstick formulation Good spreadability 29.5 60.4 30.2% with micronized red pigment Lipstick formulation Spreadability not ok; 15.9 15.8 42.3% with non-micronized pigments are not fully red pigment crushed

[0169] As can be seen from the above, micronization not only significantly improves hue and chroma, but is also very important for spreadability.

Example 9: Comparison of Carriers

[0170] The red pigment of the present invention comprises montmorillonite clay. In preliminary studies, also other carriers have been tested, using the commercial Raphanus sativus L. root extract of example 1: [0171] Sample D: 100 wt % of Raphanus sativus L. root extract; non-micronized [0172] Sample E: 50 wt % of Raphanus sativus L. root extract, 20 wt % of cellulose, 30 wt % Alun;

[0173] non-micronized; heated to 50° C. for 4 h [0174] Sample F: 50 wt % of Raphanus sativus L. root extract, 10 wt % of cellulose, 40 wt % Alun;

[0175] non-micronized; heated to 50° C. for 4 h [0176] Sample G: 50 wt % of Raphanus sativus L. root extract, 50 wt % of calcium carbonate; non-micronized [0177] Sample H: 62.5 wt % of Raphanus sativus L. root extract, 37.5 wt % of montmorillonite clay;

[0178] non-micronized [0179] Sample J: 62.5 wt % of Raphanus sativus L. root extract, 37.5 wt % of montmorillonite clay;

[0180] micronized

[0181] The above powder samples were added to the first lipstick base formulation of example 5 using the same incorporation process as described in example 5.

[0182] 2 g each of the thus obtained lipstick formulations were applied on black-and-white contrast cards using a Byko-drive G automatic film applicator (film thickness: 102 μm). The spreadability, color, hue, chroma and opacity were measured using a spectrocolorimeter Konica-Minolta 3600d.

[0183] The results were as follows:

TABLE-US-00011 CR/ opacity Spread- Hue Chroma (cover- ability L* a* b* (h) (C*) age) Sample D average 69.9 31.7 15.5 26.0 35.3 13.3% Sample E many 62.0 41.8 16.9 22.0 45.1 16.0% pigments not crushed Sample F many 66.1 30.8 10.6 19.0 32.6 13.5% pigments not crushed Sample G not all 49.4 33.5 −2.9 355.1 33.6 24.2% pigments crushed Sample H many 45.8 15.2 4.3 15.9 15.8 42.3% pigments not crushed Sample J good 44.0 52.5 29.8 29.5 60.4 30.2%

Example 10: Impact of Montmorillonite Clay in Lipstick Formulation

[0184] A second lipstick base formulation was prepared using the following ingredients: [0185] 37.5 wt % butyrospermum parkii butter [0186] 10 wt % cera alba [0187] 10 wt % caprylic/capric triglyceride [0188] 10 wt % dilinoleic acid/propanediol copolymer [0189] 5 wt % jojoba esters & Helianthus annuus seed wax & acacia decurrens flower way & polyglycerin-3 [0190] 17.5 wt % castor oil [0191] 10 wt % of pigment (with and without montmorillonite clay)

[0192] The following two pigments were tested: [0193] a. red pigment according to the present invention, as described in example 2 above [0194] b. Comparative sample B as described in example 5 above, i.e. without montmorillonite clay

[0195] The pigments were first mixed at room temperature with the castor oil using a turrax blender. The other ingredients were mixed and heated to 75° C. until the blend became homogeneous. The pigment/castor oil mixture was then added and mixed until homogeneous. The resulting mixtures were cooled down under magnetic stirring.

[0196] 2 g each of the thus obtained lipstick formulations were applied on black-and-white contrast cards using a Byko-drive G automatic film applicator (film thickness: 102 μm). Again the spreadability, hue, chroma and opacity were measured using a spectrocolorimeter Konica-Minolta 3600d.

[0197] The results were as follows:

TABLE-US-00012 CR/ Hue Chroma opacity Spreadability (h) (C*) (coverage) Red pigment a Good spreadability 29.9 62.4 29.7% (with montmorillon- ite clay) Red pigment b Spreadability 24.3 52.0 35.6% (without montmoril- slightly less good lonite clay)

[0198] As can be seen from the above, montmorillonite clay has a positive impact both on hue and chroma, and also slightly improves the spreadability.

Example 11: Home Use Test

[0199] In a home use test, 76 female volunteers in France (age 18-45) were asked to use a lipstick comprising 20% of the red pigment of the present invention at least 4 times during a 10-day test period.

[0200] The composition of the lipstick was as follows:

TABLE-US-00013 Concen- Tradename INCI Name tration Refined castor oil (Radia 6132) Ricinus Communis (castor) Seed Oil 16% (w/v) TiO.sub.2 CI 77491 (TITANIUM DIOXIDE) 1% (w/v) Red pigment of example 2 Montmorillonite, Anthocyanins, Citric acid, 20% (w/v) Maltodextrin Plurol ® Diisostearique CG Polyglyceryl-3 Diisostearate 3% (w/v) Dextrose Dextrose 0.2% (w/v) Octyldodecanol (Eutanol G) Octyldodecanol 9.48% (w/v) Coco-caprylate/caprate (Cetiol LC) Coco-caprylate/caprate 6.33% (w/v) Kahlresin 5723 Glyceryl Rosinate, Octyldodecanol 2% (w/v) Candelilla wax (Kahlwax 2039L; melting Euphorbia Cerifera (Candelilla) Wax 6.89% (w/v) point 71° C.) Carnauba wax (Kahlwax 2442L; melting Copernicia Cerifera (Carnauba) Wax 4.3% (w/v) point 84° C.) 2225 Phytowax (dropping point 73° C.) Helianthus Annuus (sunflower) Seed Cera, 1.72% (w/v) Olea Europaea (olive) Oil Unsaponifiables, Rhus Verniciflua Peel Cera/Rhus Succedanea Fruit Cera, Shorea Robusta Resin C10-18 triglycerides (Lipocire A; dropping C10-18 triglycerides 11.69% (w/v) point 35-36.5° C. Karite CP Butyrospermum Parkii (Shea) Butter 4.2% (w/v) Cegesoft ® VP (fusion point: 45° C.) Vegetable Oil, Hydrogenated Vegetable Oil, 5.16% (w/v) Euphorbia Cerifera (Candelilla) Wax Tsubaki oil deodorised olei-protect EC CAMELLIA JAPONICA SEED OIL, Polyglyceryl-3 4.28% (w/v) Diisostearate, Water, Ascorbic acid JA000040 NATROX RO E20 Helianthus annuus (Sunflower) seed oil, 0.25% (w/v) Tocopherol, Rosmarinus officinalis (Rosemary) leaf extract, Sunflower seed oil glycerides Ronaflair Boroneige SF-15 Boron Nitride 2.5% (w/v) Soothex ISA Isostearyl Alcohol, Boswellia Serrata Gum 0.5% (w/v) Fragrance FRAGRANCE 0.5% (w/v)

[0201] Feedback from the volunteers was very good: [0202] 62% of the volunteers liked the lipstick (78% of those aged 18-34) [0203] 81% of the volunteers found themselves beautiful [0204] 75% of them felt sexier [0205] Compared to other products, it was considered superior in terms of texture, perfume and taste [0206] For 53% of the volunteers, color duration met their expectations (63% of those aged 18-34) [0207] The color was found to last for 3 to 4 hours

Example 12: Purple Pigment Preparation

[0208] The Raphanus sativus L. root extract of example 1 was mixed with montmorillonite clay in a weight ratio of 5:3 in the presence of water. For instance, for a batch of 1 kg of purple pigment, 625 g of “Deodorized Red Radish Extract (Powder)” and 375 g of montmorillonite clay (“argile blanche-rosée”, ref: CosWHITE™, supplied by Argile du Velay, France) were solubilized in 900 ml of water. The pH was adjusted to about 7.5 by addition of 85 g of potassium hydroxide.

[0209] The thus obtained mixture was homogenized by stirring at room temperature and then subjected to spray drying (on a GEA Niro spray dryer) and air jet micronization. Alternatively, it would also be possible to use oven drying, without any influence on the resulting product.

[0210] Therefore, the purple pigment of the present invention is of 100% natural origin content.

Example 13: Characteristics of Purple Pigment

[0211] The purple pigment of example 12 is a purple powder. It has a mean particle size (D50) of about 2 μm to about 5 μm.

[0212] The anthocyanin content, as determined by HPLC, was from about 12 wt % to about 18 wt %.

[0213] The purple pigment has a pH of about 7.4 to about 7.8 at 1% in distilled water.

[0214] Colorimetric analysis provided the following results (at 10% in a lipstick base):

TABLE-US-00014 L* a* b* C* h 42.3 10.2 −7.7 32.0 337

[0215] Thus, the color of the purple pigment of the present invention corresponds to Pantone 518 C.

Example 14: Stability Studies

[0216] Stability at Room Temperature

[0217] The stability of a first batch of the purple pigment of example 13 in a standard lipstick base was tested at room temperature (20-21° C.), protected from light and moisture. The results were as follows:

TABLE-US-00015 Color L* a* b* DE2000 T0 32.4 6.0 −5.3 — 3 months 32.4 6.4 −5.2 0.42

[0218] Thus, the purple pigment of the present invention is perfectly stable.

[0219] It was also found to comply with the microbiological requirements (Total Plate Count=TPC; Yeasts and Mould=Y & M) for cosmetic ingredients even after 11 months.

[0220] Stability at 45° C.

[0221] The stability of a first batch of the purple pigment of example 13 in a standard lipstick base was also tested at 45° C., protected from light and moisture. The results were as follows:

TABLE-US-00016 Color L* a* b* DE2000 T0 32.3 6.4 −5.6 — 3 months 32.2 6.9 −5.5 0.54

[0222] Heat Stability

[0223] The stability of the first batch of the purple pigment of example 13 was also tested at increased temperature:

TABLE-US-00017 Color L* a* b* DE2000 rt 42.31 10.19 −7.66 — 30 min at 120° C. 42.04 10.97 −8.03 0.71 60 min at 120° C. 40.58 10.12 −6.1 1.91 90 min at 120° C. 40.74 10.37 −6.03 1.86

[0224] As can be seen from the above, the purple pigment of the present invention exhibits good stability even at high temperature. This allows for thermal debacterization if necessary.

[0225] Suntest

[0226] The color stability of a second batch of the purple pigment of example 13 was tested at 450 W/m.sup.2:

TABLE-US-00018 L* a* b* C* h DE2000 T0 42.31 10.19 −7.66 12.75 323.07 — 24 h at 450 W/m.sup.2 42.90 9.92 −6.49 11.85 326.82 1.00

[0227] Again, the purple pigment of the present invention was found to have a good stability.