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.
PHTHALATE ESTERS IN COSMETIC PRODUCTS Table II Phthalate Esters in Thirteen Commercial Cosmetic Products (PPM) No. of Product products DMP 1 DEP2 BBP3 DBP4 Body lotion 1 ND6 142 ND ND Hairspray 8 ND 81, 118, 178, 204 43 16, 38, 54 Deodorant 9 ND 38, 56, 57, 111, ND 104 681, 805, 2933 Fragrance 5 ND 5486, 8851, 9081, ND ND 11121, 38663 Skin lotion 3 ND 84 ND ND Hair gel 5 ND 53, 67 ND ND Hair mousse 5 ND 31, 56, 75, 128 ND 31, 43 Body wash 3 ND 200, 325 ND ND Shampoo ND ND ND ND Hand cream 2 ND 27 ND ND Nail enamel 6 58, 143, 15395 1136 107 25, 742, 46463, 59815 1 Dimethyl phthalate. 2 Diethyl phthalate. 5 Benzylburyl phthalate. 1 Dibutyl phthalate. 5 Diethylhexyl phthalate. 6 None detected (10 ppm). 7 Number of products containing the phthalate. 133 DEHP5 ND ND ND ND ND ND ND ND ND ND ND The source of phthalate esters in most cosmetic products is most likely the fragrance ingredient. Phthalate esters were only included on the ingredient statements of some of the nail products included in this survey. Individual fragrance ingredients are not required to be included in cosmetic product labeling (64). The Cosmetic Ingredient Review (CIR) Expert Panel, an independent panel of scientists that has been reviewing the safety of cosmetic raw materials since 197 6, has reviewed the safety of several phthalate esters used in cosmetic products. In the first review, conducted in 1985, the CIR concluded that DMP, DBP, and DEP were safe in cosmetic products at levels up to 5%, 25%, and 50%, respectively (65). In a separate review of the safety of BBP, the CIR concluded that BBP is safe at concentrations less than 1 % (66). In 2003, the CIR rereviewed the safety of phthalate esters in cosmetic products in light of reports of phthalate metabolites in human urine, and affirmed their original conclusions that the levels used in cosmetic products were safe. From 1998 to 2000, an expert panel convened by the NTP concluded that reproductive risks from exposure to phthalate esters were minimal to negligible in most cases (67). The NTP has concluded that food is the primary source of human exposure to DBP (33). In the European Union, the Scientific Committee on Cosmetics and Non-Food Products reviewed the safety of DEP and concluded it was safe in cosmetic products (68) however, the committee concluded that DBP should not be intentionally added to cosmetics (69). The significance of phthalate ester exposure from cosmetics compared to exposure from food, water, air, and plastic materials is difficult to assess. Exposure from pharmaceu- ticals must also be factored in, since high urinary levels of the metabolite of DBP have
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