PHTHALATE ESTERS IN COSMETIC PRODUCTS mAU- 3000 _ a) Standard 2500- 2000- 1500- 1000- 500- o__,___ ___� mAU 2500 2000 1500 1000 0 (b)Nail Ena DMP DEP 10 DMP BBP DBP 20 30 131 DEHP 40 min 500 0---+---�--' �-���-�------�� 0 mAU (c) Fragrance 3000 2500 2000 1500 1000 0 mAU 3000 (d) Nail Enamel 2500 2000 1500 0 10 DEP 10 10 20 30 40 min 20 30 40 min DBP 20 30 40 min Figure 1. HPLC chromatograms of (a) phthalate ester standards, (b) nail enamel, (c) fragrance product, and (d) nail enamel.
132 JOURNAL OF COSMETIC SCIENCE system was flushed with mobile phase at the beginning of each day, and after each injection the syringe was thoroughly washed with ethanol. Since DEHP is particularly persistent in the environment, and is widely used as a plasticizer, plastic materials were not used to process samples. Solvent blanks were run to confirm the absence of phthal- ates. No chromatographic responses were observed at the retention times of any of the phthalate esters. Since a wide range of phthalate ester levels are present in cosmetic products, the quantity of sample extracted was occasionally varied, depending on the expected level of phthalate ester in the product. For cosmetic products having an unknown concentration of phthal- ate ester, a preliminary analysis was made to determine the approximate level and to confirm the absence of significant chromatographic interference. Then an appropriate sample size was selected for analysis. For most products 1 g of sample was analyzed. Method accuracy was evaluated by performing recovery experiments from two hairspray products, a hand lotion, and an antiperspirant. Each product was fortified with the five phthalate esters at levels of 100 and 1000 ppm. The results are shown in Table I. Recoveries of the five phthalate esters ranged from 73% to 112%. Average recoveries for DMP, DEP, BBP, DBP, and DEHP in the four products were 91 %, 95%, 101 %, 101 %, and 92%, respectively. A survey of a variety of consumer cosmetic products for phthalate esters was conducted. Products were purchased from local stores in the Washington, DC, area, including hair care products, deodorants, lotions and creams, nail products, fragrances, and body washes. An attempt was made to purchase many of the same products analyzed by the EWG (15) to confirm the reported phthalate ester levels. The results of the analysis of 48 cosmetic products is shown in Table II. Levels less than 10 ppm are reported as not detected. Sixty-seven percent of the products analyzed contained at least one phthalate ester, while hair sprays, deodorants, nail products, and hair mousse contained two or more phthalates. The highest phthalate ester concentrations were found in nail products, with levels observed up to 59,815 ppm. DEP was the most common phthalate ester found it was present in twenty-seven products. DBP was found in ten products, while DEHP was not found in any product tested. With few exceptions, there was very good agreement between the phthalate ester levels found and those reported by the EWG. Differences observed may be due to lot variations. Table I Recovery of Phthalate Esters from Cosmetic Products* Percent recovery Product Fortification level (ppm) DMP DEP BBP DBP DEHP Hairspray A 100 90 99 99 95 84 1000 99 103 109 112 108 Hand lotion 100 89 88 97 102 73 1000 92 94 95 95 102 Antiperspirant 100 83 94 100 103 81 1000 88 95 100 99 101 Hairspray B 100 89 90 105 105 84 1000 94 98 103 100 103 * Single determination at each level.
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