PHTHALATE ESTERS IN COSMETICS 463 nail products contained phthalate ester, fi ve out of fi ve fragrances contained phthalate ester, three out of six lotions contained phthalate ester, two out of three body washes con- tained phthalate ester, and the shampoo did not contain phthalate ester. Concentrations of DBP found in 11 of the 24 nail products ranged from 123 μg/g to 62,607 μg/g. DEP was the most common phthalate ester identifi ed, with concentrations as high as 36,000 μg/g in fragrances. Twenty-four baby care products were included in the current survey. As shown in Table III, fi ve of the 24 baby-care products were found to contain DEP, which was the only phthal- ate ester found. Three out of 13 baby shampoos and body washes contained DEP at levels up to 274 μg/g, and two out of 11 baby creams, lotions, and oils contained DEP at levels up to 234 μg/g. In addition to our report in 2002 (6), two other reports have described the extraction and analysis of phthalate esters in consumer cosmetic products. De Orsi et al. (22) have de- scribed a general procedure for the analysis of phthalate esters used in their survey of 52 commercial cosmetic products, including nail polishes, enamel removers, and nail extenders marketed within the European Union. Their method utilized ultrasonic extraction of the sample with a 90/10 ethanol/water mixture for 15 minutes at 40°C. After centrifuging the sample/extract mixture, an aliquot of the clear supernatant was collected, fi ltered on a Millipore fi lter, and injected into the HPLC instrument. Chromatographic peaks were detected and quantifi ed at 254 nm. Due to the different polarity of the analytes, a gradi- ent elution technique was adopted and separation was achieved with an ethanol-water mobile phase starting at 50/50 ethanol/water and changing to 95/5 ethanol/water. A photodiode array detector was used for the evaluation of peak purity factors. The phthal- ate esters DEP, DBP, or DEHP were found in 16 of the 52 cosmetic products at concen- trations between 0.3% and 3.0%. As noted by the authors, the cosmetic products, purchased prior to January 1, 2005 and found to contain DBP or DEHP, will have to be reformulated by their respective manufacturers to comply with the EU prohibition on the use of DBP and DEHP. Shen et al. (23) described a method for the determination of phthalate esters in cosmetic products, including hair sprays, perfumes, deodorants, creams, and lotions. Phthalate esters were extracted using sonication in methanol, cleaned up with an octa carbon chain bonded silica stationary phase (C8) solid-phase extraction (SPE) column, and then separated on a C8 HPLC column with gradient elution with a methanol/water solution. Phthalate esters were detected with a diode array detector at a wavelength of 230 nm. In an analysis of Table III Phthalate Ester Concentrations Found in Baby-Care Products (μg/g) Product type Products tested DMP DEP BBP DBP DEHP Baby shampoo and body wash 13 ND* 10 ND ND ND 55 274 Baby cream, lotion, and oil 11 ND 114 ND ND ND 234 Average of duplicate injections of a single extraction (n = 1). *Not detected ( 10 μg/g).

JOURNAL OF COSMETIC SCIENCE 464 15 cosmetic products, only one was found to be free of phthalate esters. In the remaining 14 products, the phthalate esters DEP, DBP, DCHP (dicyclohexyl phthalate), and/or DEHP were found with concentrations ranging from 0.00012% to 0.53%. CONCLUSION In this report, a follow-up survey of 84 cosmetic adult-use and baby-care products for the presence of fi ve phthalate esters, DEM, DEP, BBP, DBP, and DEHP, is described. Only DEP and DBP were found in adult products, and DBP was only found in nail products. Concentrations of DBP ranged from none detected to 62,607 μg/g. Concentrations of DEP ranged from none detected to 36,006 μg/g, with DEP being the most commonly found phthalate ester. For adult-use cosmetic products, concentrations of DEP above 10 μg/g were found in fragrances, and concentrations of DBP above 10 μg/g were found in nail products. In baby-care products, DEP was the only phthalate ester found. Concen- trations of DEP ranged from not detected to 274 μg/g. DMP, BBP, and DEHP were not detected in any products. The results of this follow-up survey suggest that there is an effort to reformulate cos- metics products to reduce the use of phthalate esters in cosmetic products. Eight of the 25 products that were analyzed in our previous survey (6) no longer contained phthalate esters. Two of the 13 products that were comparable to those reported by the EWG in 2002 to contain phthalate esters (19) no longer contained phthalate esters. A comparison of the results obtained in the initial product survey (6) and this follow-up survey also suggests that there have been changes in the use of phthalate esters in some types of cos- metic products. The 2002 product survey (6) found phthalate esters in fi ve out of six of the nail products, while in this follow-up survey phthalate esters were found in 11 out of 24 nail products. No change in the use of phthalate esters was noted for fragrances. The FDA will continue to monitor adult- and baby-care cosmetic products for the pres- ence of phthalate esters as well as for any new materials that may have replaced them. The FDA does not have evidence at this time that the levels of phthalate esters present in cosmetic products are harmful to consumers as these products are currently used. If the FDA determines that a health hazard exists, the agency will advise the public and the industry, and it will take appropriate action to protect public health. REFERENCES (1) G. Latini, Monitoring phthalate exposure in humans, Clinica Chimica Acta, 361, 20–29 (2005). (2) E. Fabjan, E. Hulzebos, W. Mennes, and A. H. Piersma, A category approach for reproductive effects of phthalate, Crit. Rev. Toxicol., 36, 695–726 (2006). (3) H. J. Koo and B. M. Lee, Estimated exposure to phthalates in cosmetics and risk assessment, J. Toxicol. Env. Health A, 67, 1901–1914 (2004). (4) Cosmetic ingredient review, Annual review of cosmetic ingredient safety assessments 2002/2003, Int. J. Toxicol., 24(suppl. 1), 1–102 (2005). (5) T. Schettler, Human exposure to phthalates via consumer products, Int. J. Andrology, 29, 134–139 (2006). (6) J. C. Hubinger and D. C. Havery, Analysis of consumer cosmetic products for phthalate esters, J. Cosmet. Sci., 57, 127–137 (2006). (7) National Toxicology Program, Center for the Evaluation of Risks to Human Reproduction, NPT-CERHR Expert Panel Report on Di-n-Butyl Phthalate, October 2000.