J. Cosmet. Sci., 63, 159–176 (May/June 2012)

Determination of total lead in 400 lipsticks on the U.S. market using a validated microwave-assisted digestion, inductively coupled plasma-mass spectrometric method NANCY M. HEPP, Office of Cosmetics and Colors, Center for Food Safety and Applied Nutrition, U.S. Food and Drug Administration, College Park, MD 20740. Accepted for publication November 8, 2011. Synopsis In 2009, the U.S. Food and Drug Administration (FDA) published lead (Pb) content results from a small survey of 20 tube lipsticks with red shades using a validated inductively coupled plasma-mass spectrometric (ICP-MS) method developed by FDA chemists. The study was prompted by a media report suggesting that potential exposure to lead from lipsticks under conditions of ordinary use might be harmful. The FDA has since investigated the lead content of tube lipsticks by conducting an expanded survey that included a variety of shades and manufacturers, at varying prices. The purposes of the expanded survey were to ascertain the levels of lead in lipsticks sold on the U.S. market, to identify any categories of lipstick with elevated levels of lead, and to compare the results to those from the initial small survey. Four hundred lipsticks available on the U.S. market in the spring of 2010 were tested for total lead content using the FDA’s validated method. The analyses were performed by a private laboratory contracted by the FDA. The maximum lead level found was 7.19 mg Pb/kg. Thirteen of the 400 lipsticks were found to contain levels greater than 3.06 mg Pb/kg, the highest amount found in the initial survey. The average lead concentration found in the expanded survey was 1.11 mg Pb/kg, which was very close to the average of 1.07 mg Pb/kg found in the initial survey. Some statistically significant associations between lead level and parent company were found. The contract requirements, testing procedures, and findings from the expanded survey are described here.

INTRODUCTION

In 2009, the FDA published an initial survey of lead (Pb) content in 20 tube lipsticks with dark red shades, using a validated inductively coupled plasma-mass spectrometric (ICP-MS) method developed at the FDA (1,2). Several media reports (3–6) had generated a large number of consumer inquiries regarding the safety of lipsticks with respect to lead, and the FDA’s validated method was intended for independent assessment of the lead contamination. FDA scientists also had concerns that values reported by the media were produced using a variety of methods that could give dramatically different lead values depending on how the sample was treated. We noted that in at least one case sulfuric acid, an acid that will precipitate lead and make it unavailable for analysis, was used in extraction mixtures. 159

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Analytical techniques requiring a solubilized analyte fall into two preparation categories: (a) acid extraction of the analyte from the sample matrix, or (b) total destruction of the matrix. We chose to use a total matrix destruction technique for the validated method. Nitric acid has the desirable properties that at high temperatures can break down organic (carbon-based) molecules such as the oils and waxes in lipstick, and it also solubilizes lead as lead nitrate. Nitric acid, however, will not break down certain inorganic minerals, such as talc, mica, or titanium dioxide, which are commonly used in lipstick. In developing a method, we found that not all the lead was extracted from lipstick with nitric acid alone. After trying several total matrix destruction methods, we modified a method developed by scientists at the Cosmetics, Toiletries, and Fragrances Association (currently the Personal Care Products Council) that included a hydrofluoric acid step for breaking down the inorganic minerals (7). We then found it necessary to add an excess of boric acid to dissolve the resultant insoluble fluorides. Analyses of the resulting clear solutions by inductively coupled plasma-mass spectrometry (ICP-MS) gave reproducible lead values even under changing preparation conditions, such as using higher maximum digestion temperatures or reduced portion sizes. We used the method to determine lead in the initial survey of 20 lipsticks. Because the initial survey was small and from a limited segment of products, the FDA decided that an expanded survey of the U.S. lipstick market was needed. Since the FDA had limited time and personnel for the task, a contract laboratory was solicited to perform the study using the validated method.

EXPERIMENTAL SELECTION OF CONTRACTOR

The contractor was awarded a contract for the expanded survey on September 15, 2009, based on its demonstrated experience with lead analyses in matrices similar to lipstick and the availability of appropriate facilities, equipment, and personnel to meet technical, time, and budget criteria. Prior to analyzing the lipstick samples, the contractor was asked to demonstrate its ability to obtain values that agreed with those for three reference lipsticks, as well as to meet specific performance criteria regarding limit of detection, quality control, and precision.

LIPSTICK SAMPLING

Lipsticks for the expanded survey were selected by choosing manufacturers, brands, and shades that reflected the products currently on the market. This was accomplished by proportioning the number of lipsticks chosen from each brand to its market share using data from the 2008 Euromonitor Report (8). A few additional lipsticks were selected from niche markets in an effort to capture lipsticks with unusual characteristics. A total of 400 lipsticks with a variety of shades, with no particular targeted colors, were selected from 24 parent companies. One pair of lipsticks per manufacturer with the same lot number (and therefore the same shade) was collected as an additional test of lot homogeneity. Each of the 400 lipsticks was tested in duplicate.

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APPARATUS

Lipsticks were digested in CEM EasyPrepTM vessels on a CEM MARS microwave digestion system (CEM Corporation, Matthews, NC). The analytical solutions were stored in metal-free grade polypropylene centrifuge tubes, with additional acid cleaning to remove contamination (50 ml, Tyco Healthcare Group, Mansfield, MA, and 15 ml, VWR International, Radnor, PA). Lead analyses were performed on a Perkin Elmer Elan 6000 with DRC II ICP-MS (Perkin Elmer, Shelton, CT). REAGENTS

High purity (18 MΩ) deionized water was used throughout. Lead standard (0, 0.01, 0.02, 0.04, 0.08, 1.25, 2.50, 5.00, 12.50, and 25.00 μg Pb/l), lead stock (0.100 and 1.00 mg Pb/l), and platinum internal standard (0.4 mg Pt/l) solutions were prepared from commercial ICP-MS grade single-element analyte solutions (CPI International, Santa Rosa, CA). Trace metal grade nitric acid (EMD Chemicals, Gibbstown, NJ) was used for sample, stock, and standard solutions. Hydrofluoric acid (Fisher Scientific, Pittsburgh, PA) was used in the sample solutions. Boric acid (Puratronic grade, Alfa Aesar, Ward Hill, MA) was used to prepare 4% boric acid solution. A 0.100 mg Pb/kg in oil stock solution was prepared from 1000 mg Pb/kg organo-metallic standard serially diluted to 10.00 and then to 0.100 mg Pb/kg with base oil 20 (organo-metallic lead standard and base oil, both from Spex CertiPrep, Inc., Metuchen, NJ). Nitric acid (1%, v/v) was used for preparing calibration standards and analytical solutions. Water standard reference material NIST SRM 1643e (National Institute of Standards and Technology, Gaithersburg, MD) containing 19.15 ± 0.20 mg Pb/kg, diluted 1/10 with 1% nitric acid, was used as a secondary standard to check ICP-MS performance.

METHOD

The protocol was consistent with the FDA’s validated method (1), and continued reliability of the results was verified by using specific quality control procedures, as follows: • Weigh and transfer 0.3 ± 0.1 g of lipstick to a digestion vessel liner. • Add 7 ml of nitric acid and 2 ml of hydrofluoric acid to the lipstick in the liner. • Seal and heat the vessels in the microwave digestion oven. Ramp the temperature over 20 minutes to 130°C and hold for three minutes, then continue to ramp the temperature over 20 minutes to 200°C and hold for 30 minutes. Allow the samples to cool to less than 50°C. • Vent and open the vessels in a fume exhaust hood. • Add 30 ml of 4% boric acid solution to each. • Reseal and heat the vessels in the microwave digestion system. Ramp the temperature over 20 minutes to 170°C and hold for ten minutes. Cool, vent, and open the vessels in a fume exhaust hood. • Quantitatively transfer the contents of the digestion vessels to 50-ml centrifuge tubes and dilute to 50 ± 0.25 ml with water. • Include two method blanks in each digestion batch to assess contamination.

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• Include one method blank fortified with organic lead in oil (low-level organic lead fortification solution) in each digestion batch. • Include one method blank fortified with inorganic lead (low-level inorganic lead fortification solution) in each digestion batch. • Prepare each lipstick sample in duplicate.

ICP-MS ANALYSIS

Internal standardization was performed using a 195Pt isotope. The analytical run began with a seven-point standard curve between 0.010 μg Pb/l and 25 μg Pb/l, with continuing calibration verification standards run every 15 samples. The daily calibration standard curves were calculated using linear regression (ELAN software). The instrument was tuned in the “normal” (no gas) mode to meet specifications for sensitivity, oxide ratio, and doubly charged ratio as detailed by Perkin Elmer. Analytical solutions and standards were merged online with the internal standard solution via a T-fitting before the nebulizer. The method was set up to quantify lead using a sum of the isotopes 206,207,208Pb to account for isotopic variation between samples and standards. The 195Pt isotope was measured for internal standardization. Prepared samples (analytical solutions) were analyzed using a dilution of 1/20 in 1% (v/v) nitric acid relative to calibration standards using linear regression (y = ax + blank). No analytical solutions had internal standard signals that differed by more than 40% relative to the calibration blank.

QUALITY CONTROL

The correlation coefficient for the standard curve was greater than 0.997 in all cases. Calibration was verified by analyzing a calibration blank and two quality control (QC) solutions (secondary inorganic lead stock solution and lead in water reference solution) immediately after calibration and after every 15 analytical solutions. The QC solution recovery was between 90% and 110%. One analytical solution from each digestion batch was diluted 1/40 with 1% nitric acid and compared with the same solution diluted 1/10 to evaluate matrix effects. Any analytical solutions with lead levels above the highest standard were further diluted to within the calibration range to determine the lead concentration.

STATISTICAL COMPARISON OF MEAN LEAD VALUES AMONG COMPANIES

Seven parent companies with 18 or more lipsticks from each company made up nearly 80% of the samples (319 out of 400 lipsticks). These seven companies (number of lipsticks) were Companies A (77), C (21), D (41), E (20), F (18), G (117), and H (25). To test for significant differences among companies, an analysis of variance (ANOVA) was performed using the mean lead value data. The log-transformed data were used in the ANOVA because they were more normally distributed. Since the overall ANOVA test was significant at p ≤ 0.05, we performed a

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pair-wise comparison using a least significant difference test to statistically compare the mean lead values for each company.

RESULTS

The lead values for the 400 lipsticks are reported in the Appendix. The mean or average lead concentration found in the 400 lipsticks tested was 1.11 mg Pb/kg, very close to the average of 1.07 mg Pb/kg obtained in the initial survey (1). The standard deviation was 0.97 mg Pb/kg. The results ranged from the detection limit of 0.026 mg Pb/kg to the highest value of 7.19 mg Pb/kg. (The average of 1.11 mg Pb/kg is the same whether or not the three lipsticks with lead values below the detection limit are included as “0 mg/kg” or as “0.026 mg/kg.” The initial survey did not include any lipsticks with lead values below the detection limit.) The median was 0.89 mg Pb/kg. The mean is higher than the median because a few lipsticks had high lead values, but most (247) lipsticks had lead values less than the mean value. More than 350 of the 400 lipsticks (88%) contained less than 2 mg Pb/kg, as shown in Figure 1. The 99% upper confidence limit (one-tail) value is 3.36 mg Pb/kg. Eleven samples (2.75%) were found to be above that limit, but since two samples were a pair of lipsticks with the same shade and lot number, only ten lipsticks (2.5%) were found to be above the limit. The results for the ten lipsticks with lead levels above the 99% upper confidence limit are shown in Table I in order of descending lead value. Parent company designations are assigned by first appearance in the Appendix. Brand designations distinguish brands within each parent company. Shade numbers distinguish shades within each brand. Five of the ten lipsticks that exceeded this limit were from Company A. The mean, median, and 99% upper confidence limits for companies with more than ten lipsticks and for all lipsticks (including the companies with less than ten lipsticks) are shown in Table II. Company B, a company with high lead values, does not appear separately in Table II because the number of lipsticks tested was less than ten. The difference between mean and median lead values for some companies, such as Companies C and D, is very small, whereas the difference between mean and median values for other companies, such as Companies A, E, and F, is large. Large differences indicate that a few lipsticks have unusually high values, which influence the mean more than

Figure 1. Lead content in lipstick samples.

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JOURNAL OF COSMETIC SCIENCE Table I Lipsticks Containing More Than 3.36 mg Pb/kg

Parent company (manufacturer)

Brand

Shade

Lead (Pb) mg/kg

A

a

1

7.19

A B C B A A C A F

b a a a b b b a a

1 1 1 2 2 3 1 2 1

7.00 4.93 4.92 4.89 4.45 4.41 4.28 4.23 4.12 and 4.06

Lipstick results are reported in order of descending lead value. Parent company designations were assigned by first appearance in the Appendix. Brand designations distinguish brands within each parent company. Shade numbers distinguish shades within each brand.

the median. The individual 99% upper confidence limits for Companies A, C, and F exceed the limit for all lipsticks because of large variations in lead values for lipsticks in those companies. Notably, Company A’s distribution of lead values is skewed by its five high values.

QUALITY CONTROL RESULTS

To assess matrix effects, the contractor was asked to perform serial dilutions on one analytical solution in each digestion batch. Of the 100 serial dilutions performed, eight

Table II Mean and Median Pb Values for Companies with More Than Ten Lipsticks Company (number of lipsticks) A (77) C (21) D (41) E (20) F (18) G (117) H (25) I (11) All lipsticks (includes companies with < 10 lipsticks)

Mean Pb mg/kg

Median Pb mg/kg

99% Upper confidence limit

1.25 2.01 1.68 1.04 1.47 0.66 1.00 0.78

0.93 2.00 1.70 0.58 1.07 0.56 0.86 0.70

4.35 5.00 3.31 3.25 4.48 1.77 2.14 1.47

1.11

0.89

3.36

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lipsticks resulted in relative percent differences (RPD) of more than 10%, but only two lipsticks exhibited an absolute difference of more than 0.30 mg Pb/kg, suggesting few influences from the matrix. Repeatability was demonstrated by preparing lipsticks in duplicate. The average value of differences between duplicate preparations was less than the estimated precision of the method (0.05 mg Pb/kg). As another check of method performance and sample homogeneity, the contractor was asked to collect a second lipstick of the same shade and lot number from each manufacturer. Of these pairs, 18 of the 19 results agreed within 0.10 mg Pb/kg and therefore showed good method repeatability and homogeneity of the lipsticks. One lipstick initially showed a difference of more than 3.0 mg Pb/kg between tubes. However, a repeat analysis showed agreement within 0.3 mg Pb/kg, and the initial difference was attributed to a preparation batch with mislabeled analytical solutions. The discrepancy prompted the FDA to follow up with several additional repeat analyses and preparations.

CHECK ANALYSES

To make sure that correct values were reported, the contractor reanalyzed 10% of its analytical solutions and the FDA repeated the preparations and analyses of several lipsticks, including the lipsticks with the 15 highest lead values. This process not only identified the mislabeled preparation batch described above, but also revealed a second preparation batch whose lead values were calculated with an incorrect dilution factor. The data were corrected accordingly.

STATISTICAL COMPARISON OF MEAN LEAD VALUES AMONG COMPANIES

We found that Company G lipsticks had lead values significantly lower than those from each of the other six companies. Lipsticks from Companies A, E, and H had significantly lower mean lead values than lipsticks from both Companies C and D, but their mean lead values were not significantly different from each other. The mean lead value for Company F lipsticks was only significantly different (higher) than Company G’s.

DISCUSSION

The FDA is aware that two other groups have reported results for lead in lipsticks using the FDA’s method. One group from the U.S. analyzed 56 lip products including lipsticks, lip glosses, moisturizing sticks, and lip stains, and reported an average of 0.9932 mg Pb/kg (9). An E.U. group surveyed 81 lipsticks and 32 lip glosses purchased in the E.U. in 2010 and 2011 and found an average lead content of 0.86 mg Pb/kg for the lipsticks, with a range of 0.05 to 3.75 mg/kg (10). The lip glosses contained less lead (averaging 0.44 mg Pb/kg), which the authors considered to be a result of their lower pigment content. In our previous work (1), we similarly attributed higher lead content to higher mineral or pigment content. The authors illustrated the lower lead content of the

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lip glosses by plotting lead content versus product type. The curve for lip glosses fell about 1 mg Pb/kg below the curve for lipsticks. The E.U. group looked for trends relating lead content to lipstick shade and found that the lead content in the pink shades was highest, followed by purple, and then red. The authors did not provide an explanation for this trend, but it is possible to understand the trend for higher lead in shades with higher levels of mineral pigments acting as lightening toners for the darker red shades. We found it difficult to categorize the lipstick shades we surveyed because the hues blend from one color to another, and we did not attempt to find associations between lead content and shade. Lipsticks with lead content greater than 3.36 mg Pb/kg had a variety of shades. The E.U. group also compared lead content to lipstick price but did not find any trend. We made no attempt to associate lead content with price, in part because the same shades are available at multiple prices. The higher mean lead values for Companies C and D may be a reflection of the source of raw materials, but this would need further investigation and proprietary information from the lipstick manufacturers. It is interesting to note that one manufacturer (Company G) was able to attain significantly lower lead values than the other companies (See Table II and the statistical analyses). Both the U.S. and E.U. groups found an average lead content in lipsticks that is consistent with the average of 1.11 mg Pb/kg determined in this study. The E.U. group also concluded that lip products in the E.U. normally contain lead in the range of 1–2 mg Pb/kg. Our results are consistent with this finding, as is evident from Figure 1, which shows that nearly 90% of the lipsticks we surveyed contain less than 2 mg Pb/kg. CONCLUSIONS

The mean lead content found in lipsticks from the initial (1.07 mg Pb/kg) and expanded (1.11 mg Pb/kg) surveys was approximately the same. The median lead content from the expanded survey was 0.89 mg Pb/kg. Only ten lipsticks (2.5%) in the expanded survey, and none in the initial survey, were found to contain lead above the 99% upper confidence limit of 3.36 mg Pb/kg. Some statistically significant associations between lead level and parent company were found.

ACKNOWLEDGMENTS

I thank the FDA’s William Mindak for his guidance and advice on analytical aspects, Dennis Ruggles for performing statistical calculations, Beth Meyers for editing the large table of lipstick and lead results, Julie Barrows for significant editorial advice, Patricia Hansen for contract advice, and John Gasper for coordinating efforts between the FDA and the contractor. REFERENCES (1) N. M. Hepp, W. R. Mindak, and J. Cheng, Determination of total lead in lipstick: Development and validation of a microwave-assisted digestion, inductively coupled plasma-mass spectrometric method, J. Cosmet. Sci., 60, 405–414 (2009).

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(2) U.S. Food and Drug Administration, Lipstick and Lead: Questions and Answers, accessed September 2011, http://www.fda.gov/cosmetics/productandingredientsafety/productinformation/ucm137224. htm (3) Campaign for Safe Cosmetics, A Poison Kiss: The Problem of Lead in Lipstick, October 2007, accessed September 2011, http://safecosmetics.org/article.php?id=327 (4) R. Paige, Dangerous Levels of Lead in Lipstick, Lip Gloss? CBS Los Angeles, May 17, 2006, accessed July 2008, no longer accessible, http://cbs2.com/consumer/Lipstick.Lip.Gloss.2.516979.html (5) A. Meyer, Pretty Little Lie, News Channel 4, Oklahoma City, May 19, 2006, accessed July 2008, no longer accessible, www.kfor.com/global/story.asp?s=4908398 (6) B. Thompson, Is Lead Inside Lipstick? WPXI, Pittsburgh, PA, July 24, 2006, accessed September 26, 2008, no longer accessible, http://www.wpxi.com/print/9566833/detail.html (7) Cosmetics, Toiletries, and Fragrances Association, Determination of Lead Content of Finished Cosmetics and Raw Materials by Closed-Vessel Microwave Digestion Graphite Furnace Atomic Absorption Spectrometry, CTFA Lead Analysis Task Force, November 19, 1997. (8) “Lip Products Brand Shares by Retail Value 2004–2007,” in Cosmetics and Toiletries in the U.S. (Euromonitor International Ltd, London, May 2008), Table 64, pp. 78–79. (9) P. Atkins, H. Lang, W. Driscoll, and L. Ernyei, Analysis of lipstick for toxic elements using ICP-MS, 2011 Pittsburgh Conference on Analytical Chemistry and Applied Spectroscopy, Atlanta, Georgia, March 13–18, 2011 (poster presentation). (10) P. Piccinini, M. Piecha, and S. Fortaner Torrent, Results of European survey on lead in lipsticks, Technical Note LB-NA-24886-EN-N, European Commission, Joint Research Centre, Institute for Health and Consumer Protection (European Union, August 2011). APPENDIX Lead (Pb) Results for 400 Lipsticks from 24 Parent Companies, Purchased between February and July 2010 Parent (manufacturer)

Brand

A A B C B A A C A F F D J E A D K D J D C F L E

a b a a a b b b a a a a a a b a a a a a b a a a

Lead (Pb) mg/kg 7.19 7.00 4.93 4.92 4.89 4.45 4.41 4.28 4.23 4.12 4.06 3.32 3.12 3.08 2.87 2.84 2.81 2.81 2.80 2.77 2.74 2.71 2.68 2.59 (Continued)

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Brand

Lead (Pb) mg/kg

C C D D C D C A G C F C D K D E C D L D H M G G C C A N F H E C A C C D O D N P D B D D H

b b a a b a b c a a a b a a a a a b a a a a a b b b b a a a a b a a b a a a a b a a a b a

2.56 2.52 2.52 2.44 2.42 2.40 2.28 2.28 2.28 2.27 2.27 2.26 2.25 2.24 2.24 2.23 2.22 2.21 2.18 2.12 2.09 2.08 2.08 2.07 2.00 2.00 2.00 1.98 1.98 1.96 1.95 1.94 1.94 1.93 1.92 1.91 1.88 1.88 1.88 1.86 1.85 1.84 1.84 1.82 1.82

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APPENDIX Continued Parent (manufacturer)

Brand

Lead (Pb) mg/kg

D A D G A C Q D D M E A A D D R R A A B A A D G F P D D P F G G H A A A D E A A A D E H

a b a a a b a a a a a b a a b a a b b a b a a a a a a a b a b a a a a a a a b b a b a a

1.81 1.80 1.80 1.78 1.78 1.76 1.76 1.75 1.75 1.74 1.73 1.72 1.71 1.70 1.69 1.69 1.69 1.69 1.69 1.69 1.63 1.61 1.61 1.57 1.57 1.56 1.55 1.54 1.53 1.53 1.50 1.49 1.49 1.48 1.47 1.46 1.46 1.45 1.45 1.44 1.41 1.40 1.39 1.39 (Continued)

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Brand

Lead (Pb) mg/kg

S A F G A S G D A G G G D G A H D Q D H G G T D A I A T G A D T L U G H T G A D A I F O A G

a b a a a a a b c a c a a d c a a a b a c c a b b a c a c c a a a a c a a c c b c a a a b a

1.38 1.38 1.38 1.37 1.37 1.36 1.35 1.34 1.34 1.34 1.33 1.32 1.32 1.31 1.31 1.30 1.28 1.27 1.26 1.26 1.24 1.24 1.23 1.22 1.21 1.20 1.20 1.19 1.18 1.18 1.18 1.18 1.17 1.17 1.15 1.15 1.15 1.13 1.13 1.12 1.11 1.10 1.10 1.08 1.08 1.08

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APPENDIX Continued Parent (manufacturer)

Brand

Lead (Pb) mg/kg

E G A D I G A D G A F P U H G G A G H G A G G G B D F G E A V G H F G A H A Q A G A I G

a c c a a b b a a a a b a a a c c a a a c e c a a a a a a a a a a a c c a a a a a a a a

1.07 1.07 1.07 1.06 1.05 1.04 1.04 1.04 1.03 1.03 1.03 1.02 1.02 1.02 1.01 1.00 1.00 1.00 0.97 0.96 0.96 0.95 0.95 0.95 0.95 0.95 0.95 0.94 0.93 0.93 0.93 0.92 0.92 0.92 0.91 0.91 0.91 0.91 0.90 0.90 0.89 0.89 0.88 0.88 (Continued)

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JOURNAL OF COSMETIC SCIENCE APPENDIX Continued Parent (manufacturer)

Brand

Lead (Pb) mg/kg

G Q A H O I G G G H G P A A G F G G U H A G G G G K A A C G H G G G H A A H F I H V A A A G

c a b H a a c a a a c a b b c a a a a a c e a d a a b a a a a c a a a c b a a a a a c c b a

0.86 0.86 0.86 0.86 0.85 0.84 0.84 0.84 0.83 0.83 0.82 0.82 0.82 0.82 0.81 0.81 0.80 0.80 0.80 0.80 0.79 0.78 0.78 0.78 0.77 0.76 0.76 0.76 0.75 0.75 0.75 0.74 0.74 0.74 0.74 0.73 0.73 0.72 0.72 0.70 0.70 0.70 0.69 0.69 0.69 0.69

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APPENDIX Continued Parent (manufacturer)

Brand

Q D G A T V H D G G H F G G H H I I A E E I G G H E G E A G I G O G A G A A I G G E C P G

a a a b a a a a a a a a a a a a a a a a a a c c a a a a a b a a a c c a a c a a a a a b b

Lead (Pb) mg/kg 0.68 0.68 0.67 0.66 0.66 0.64 0.63 0.63 0.62 0.62 0.61 0.61 0.60 0.60 0.60 0.60 0.59 0.59 0.59 0.58 0.58 0.58 0.58 0.57 0.57 0.56 0.56 0.55 0.55 0.54 0.53 0.53 0.52 0.52 0.52 0.52 0.52 0.51 0.50 0.50 0.50 0.49 0.49 0.48 0.48 (Continued)

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JOURNAL OF COSMETIC SCIENCE APPENDIX Continued Parent (manufacturer)

Brand

Lead (Pb) mg/kg

E U W G G G D B K G G A G G G G C G G G G G A B G E G G O T G B F W G P G E A G F G A A H

a a a c a a a a a c c c a a e c a a c d a a a a a a a a a a a a a a a a a a b a a c c b a

0.47 0.47 0.47 0.46 0.45 0.45 0.44 0.44 0.43 0.43 0.43 0.43 0.41 0.41 0.40 0.40 0.40 0.40 0.39 0.39 0.39 0.39 0.39 0.39 0.38 0.37 0.37 0.37 0.35 0.35 0.33 0.32 0.32 0.32 0.31 0.31 0.31 0.30 0.30 0.30 0.30 0.29 0.29 0.29 0.29

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APPENDIX Continued Parent (manufacturer)

Brand

Lead (Pb) mg/kg

C A D G A G A G G G G A G A B G G W E G G A A G E C G A Q A G G F A U G W E G G G P A G

b a a c c a c c a a c c a a a e c a a c d c c a a b c c a b a a a b a a a a e a a b b a

0.28 0.28 0.28 0.27 0.27 0.27 0.26 0.25 0.25 0.24 0.23 0.23 0.23 0.23 0.23 0.22 0.22 0.22 0.21 0.20 0.20 0.20 0.20 0.20 0.18 0.18 0.17 0.17 0.16 0.16 0.15 0.15 0.15 0.14 0.13 0.13 0.13 0.12 0.12 0.12 0.11 0.08 0.08 0.08 (Continued)

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JOURNAL OF COSMETIC SCIENCE APPENDIX Continued Parent (manufacturer)

Brand

Lead (Pb) mg/kg

G G G T G G L L U G X G G X G A W

a c c a e e a a a a a a a a c b a

0.08 0.07 0.07 0.07 0.06 0.06 0.06 0.05 0.05 0.05 0.05 0.04 0.03 0.03