PHTHALATE ESTERS IN COSMETICS 461 and then extracted as described above. To avoid sample contamination by environmental sources of phthalate esters, all glassware was thoroughly cleaned and rinsed with DI water and ethanol before use. Contact with plastics that could contain phthalate esters was avoided. HPLC ANALYSIS Analyses were carried out on an Agilent 1100 series HPLC. Chromatographic separation was achieved using a Partisil ODS-3, 5-μm, analytical column (250 mm by 4.6 mm ID.) and a solvent program starting initially with 50% water, 34% acetonitrile, 13% 2-propanol, and 3% methanol that was changed linearly (35 minutes) to 15% water, 55% acetonitrile, 25% 2-propanol, and 5% methanol and was held for an additional ten minutes. The fl ow rate was 1.0 ml/min. The system was then gradually returned to the starting gradient and pressure for the next sample (ten minutes). Peaks were detected at 230 nm. Phthalate esters were determined in sample extracts and standards by duplicate injection of 20 μl. External standard calibration was used to quantitate the phthalate esters. Average peak areas were calculated for each phthalate ester, and the amount of analyte was determined using a four-point calibration curve. The limit of quantitation (LOQ), defi ned as ten times the baseline noise, ranged from 1 μg/g to 10 μg/g. Values less than the LOQ were reported as not detected. The recovery of phthalate esters from antiperspirant and nail color cosmetic products was determined by fortifying products with 100 μg/g and 1,000 μg/g of each ester followed by extraction and HPLC analysis as described above. RESULTS AND DISCUSSION The present follow-up survey was initiated to fi nd out if any of the products analyzed previously had been reformulated to reduce or eliminate phthalate esters. To verify that the analytical method was still valid, a small recovery study was conducted. As shown in Table I, recoveries for the fi ve phthalate esters DEM, DEP, BBP, DBP, and DEHP ranged from 88% for DBP spiked at 100 μg/g in an antiperspirant to 104% for DBP spiked at 100 μg/g in a nail color. Both adult- and baby-care cosmetic products were included in the study. As shown in Table II, 31 of the 60 adult-use cosmetic products analyzed were found to contain a Table I Mass Recovery of Phthalate Esters from Cosmetic Products Product Spike (μg/g) Percent recovery for each phthalate ester DMP DEP BBP DBP DEHP Antiperspirant 100 94.8 97.3 98.9 88.0 97.6 1000 98.6 96.8 97.1 94.0 100.5 Nail color 100 99.9 103.1 90.8 104.4 100.8 1000 98.4 96.7 94.3 92.8 96.6 Average of duplicate injections of a single determination (n = 1) of each spike level. Mass recovery = (μg/gfound ÷ μg/gspiked) × 100%.

JOURNAL OF COSMETIC SCIENCE 462 phthalate ester. DEP was the most common phthalate found and was present in 21 prod- ucts. DBP was only found in nail products and was present in 11 of the 24 nail products analyzed. Among the 25 products comparable to those analyzed previously (6), eight no longer contained phthalate esters. Among the 13 products comparable to those previ- ously reported by the EWG to contain phthalate esters (19), two no longer contained phthalate esters. In terms of the distribution of phthalate esters in the different adult-use product types, four out of 12 deodorants contained phthalate ester, four out of seven hair products con- tained phthalate ester, 11 out of 24 nail products contained phthalate ester, all 11 fra- grances contained phthalate ester, one out of three lotions contained phthalate ester, and neither of the two body washes or the one shampoo contained phthalate ester. In the previous FDA survey results in 2002 (6), eight out of nine deodorants contained phthalate ester, 14 out of 18 hair-care products contained phthalate ester, six out of six Table II Phthalate Ester Concentrations Found in Adult-Use Cosmetic Products (μg/g) Product type Products tested DMP DEP BBP DBP DEHP Lotion 3 ND* 133 ND ND ND Hair spray, 7 ND 80 ND ND ND gel, mousse 153 181 316 Deodorant 12 ND 164 ND ND ND 316 1433 2699 Fragrance 11 ND 1328 ND ND ND 3036 5247 6107 8052 8669 10145 23410 31116 34479 36006 Body wash 2 ND ND ND ND ND Shampoo 1 ND ND ND ND ND Nail polish, 24 ND ND ND 122 ND color, enamel 123 374 50278 55489 58765 59852 59992 60475 61065 62607 Average of duplicate injections of a single extraction (n = 1). *Not detected ( 10 μg/g).