Simultaneous determination of 19 phthalate esters in cosmetics using gas chromatography-mass spectrometry
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- Ἀσκληπιός Μεταξάς
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1 Vol. 30 No. 3 March 2012 Chinese Journal of Chromatography 273 ~ 279 DOI /SP. J * GC-MS m /m v /v GC- MS μg /g ~ μg /g RSD n = μg /g ~ μg /g 6 19 PAEs PAEs - O658 A Simultaneous determination of 19 phthalate esters in cosmetics using gas chromatography-mass spectrometry LIANG Jing 1 3 ZHUANG Wan e 1 WEI Danqi 2 OU Yan 3 GONG Zhenbin 1* 1. State Key Laboratory of Marine Environmental Science Xiamen University Xiamen China 2. Fujian Food and Drug Administration Fuzhou China 3. Fareast Testing & Technology Services Co. Ltd. Fujian Quanzhou China Abstract A method was developed for the simultaneous determination of 19 phthalate esters PAEs at trace level in cosmetics by solid phase extraction SPE purification and gas chromatography-mass spectrometry GC-MS detection. The PAEs were extracted from cosmetic samples by dichloromethane with ultrasonic-assisted technique purified by an SPE column packed with silica gel and neutral alumina 2 3 m /m with the elution of 20 ml of mixed solvent of ethyl acetate-hexane 8 2 v /v. Qualitative and quantitative analysis were carried out by GC-MS in full scan and selected ion monitoring modes. The retention time of quantitative ions and the abundance ratio of characteristic ions were applied to rapidly and accurately identify each analyte so as to prevent the occurring of possible mistakes from complex matrix intervention. Under optimized conditions the average recoveries for a shampoo sample spiked with the standards at μg /g were in the range of and and the relative standard deviations RSDs for the 19 PAEs were less than n = 6 at the spiked level of 0. 1 μg /g. The limits of detection LODs as 3 times of standard deviation were between μg /g for diisopentyl phthalate and μg /g for diisobutyl phthalate. The method was successfully applied to the determination of the PAEs in 6 types of cosmetics. It is expected to promote the determination of the PAEs in other cosmetics with different matrices. Key words gas chromatography-mass spectrometry GC-MS phthalate esters PAEs cosmetic phthalate esters PAEs 1 PAEs 2 PAEs *. Tel zbgong@ xmu. edu. cn
2 bis 2-ethoxyethyl phthalate 3 4 BEEP di-n-hexyl phthalate DnHP butyl benzyl PAEs phthalate BBP 2- di WHO ethylhexyl phthalate DEHP PAEs di-n-heptyl phthalate DHP 76 /768 /EEC 2007 dicyclohexyl phthalate DCHP PAEs di-n-octyl phthalate DnOP 18 PAEs diundecyl phthalate DUP Sigma-Aldrich IS 1 GC-MS di-n-butyl phthalate PAEs 15 6-D4 DBP-D Sigma-Aldrich PAEs di 2-ethylhexyl phthalate D4 DEHP PAEs D Dr. Ehrenstorfer Gmbh - SPE GC-MS 19 PAEs E PAEs PAEs 7890A GC-5975C MS mg /L Agilent Technologies KQ-400KDE DBP-D4 DEHP-D4 TGL-10B 100 mg /L DC-12H 4 Tedia 10 mg /L Fisher ~ g ml h dimethyl phthalate DMP Dr. Ehrenstorfer Gmbh PAEs 40 ~ min r /min 5 min diethyl phthalate DEP 1 2 diallyl phthalate DAP 1. 0 ml dipropyl phthalate DPP diisobutyl phthalate DIBP 800 mg mg di-n-butyl phthalate DBP bis 4-methyl-2-pentyl phthalate 5 ml v /v BMPP diisopentyl phthalate SPE 20 ml DIPP 2- bis 2-methoxyethyl phthalate DMEP v /v pentyl isopentyl phthalate PIPP SPE PAEs 2 ml /min di-n-pentyl phthalate DnPP DBP-D4 DEHP-
3 D4 50 μl 0. 5 ml GC-MS PAEs 1. 0 μl DB-35 MS m mm μm kpa 1. 0 min > He 1. 0 ml /min /min /min /min min electron DEHP-D4 1 ionization EI 70 ev 230 DBP DEHP / Scan PAEs /SIM PAEs 3. 5 min 1 ± PAEs 2 Table 1 PAE Retention times t R characteristic ions and their abundance ratios of 19 PAEs and 2 internal standards t R /min Characteristic ion m /z Abundance ratio DMP * DEP * DAP * DPP * DIBP * DBP-D4 IS * 100 DBP * BMPP * DIPP * DMEP * PIPP * DnPP * BEEP * DnHP * BBP * DEHP-D4 IS * DEHP * DHP * DCHP * DnOP * DUP * * Quantitative ion. IS internal standard h 19 PAEs 1 1 DBP DBP-D4 DEHP PAEs 1 ~ 13 PAEs DBP-D4 14 ~ 21 PAEs DE- HP-D μg /g DCM EtAc Met Hex - Ace 1 1 v /v PAEs v /v GC-MS PAEs 2 2 PAEs 0. 5 μg /g 3 a 10 ml 1 30 min b 20
4 a 19 PAEs b 0. 5 μg /g SIM Fig. 1 Selected ion monitoring chromatograms of a a mixed solution of 19 PAEs standards and b a shampoo sample spiked with 19 PAEs standards at 0. 5 μg /g Peaks 1. DMP 2. DEP 3. DAP 4. DPP 5. DIBP 6 and 7. DBP and DBP-D4 IS 8. BMPP 9. DIPP 10. DMEP 11. PIPP 12. Dn- PP 13. BEEP 14. DnHP 15. BBP 16 and 17. DEHP and DEHP-D4 IS 18. DHP 19. DCHP 20. DnOP 21. DUP. b 2 PAEs 3 3 PAEs Fig. 2 Efficiencies of extraction by different solvents for PAEs spiked in a shampoo sample Fig. 3 Influences of three different extraction procedures on the recoveries of PAEs spiked in a shampoo sample Extraction solvents Hex n-hexane DCM dichloromethane Met methanol EtAc ethyl acetate Hex-Ace n-hexane-acetone 1 1 v /v. ml 2 30 min 10 ml /15 min / c 30 ml 3 a. 10 ml /30 min /time one time b. 10 ml /15 min /time two times c. 10 ml /10 min /time three times min 10 ml /10 min / a b c 3
5 μg /g g 4 6 m / m PAEs v /v 20 ml PAEs 5 2 g 4 6 m /m - 20 ml 8 2 v /v PAEs Fig. 5 Influences of different ratios of EtAc-Hex as eluents on the recoveries of PAEs spiked in a shampoo sample 4 - PAEs Fig. 4 Influences of mixture ratio of silica gel and neutral alumina as sorbents on the recoveries of PAEs spiked in a shampoo sample ~ 10 mg /L μg /g μg /g 0. 1 μg /g RSD 19 PAEs r PAEs ~ RSD 4. 3 ~ LOD μg /g DIPP ~ μg /g DIBP 2 DIBP DBP DEHP 3 PAEs μg /g μg /g PAEs 6 x 25 ml 10 y 1. 0 μg /g r DBP DEHP μg /g 6 3 LOD μg /g ~ μg /g 6 PAEs 5
6 PAEs PAEs 2 19 PAEs RSD LOD Table 2 Calibration equations correlation coefficients r spiked recoveries relative standard deviations RSDs and limits of detection LODs of 19 PAEs PAE Calibration equation 1 r Spiked recovery / 0. 1 μg /g 0. 5 μg /g 2. 0 μg /g RSD n = 6 2 / LOD S /N = 3 3 / DMP y = x DEP y = x DAP y = x DPP y = x DIBP y = DBP y = x BMPP y = x DIPP y = x DMEP y = x PIPP y = x DnPP y = x BEEP y = x DnHP y = x BBP y = x DEHP y = x DHP y = x DCHP y = x DnOP y = x DUP y = x x the spiked level y the peak area ratio of quantitative ions of analyte and IS. 2 The RSDs were obtained from the spike test at 0. 1 μg /g. 3 The LODs were obtained from the spike test at μg /g PAEs 1. 0 μg /g Table 3 Contents of 19 PAEs in smoothing toner mask powder and hand cream samples and recoveries of 19 PAEs spiked in 3 cosmetic samples at 1. 0 μg /g PAE Smoothing toner Mask powder Hand cream DMP n. d n. d DEP n. d DAP n. d n. d n. d DPP n. d n. d n. d DIBP DBP n. d n. d n. d BMPP n. d n. d n. d DIPP n. d n. d n. d DMEP n. d n. d n. d PIPP n. d n. d n. d DnPP n. d n. d n. d BEEP n. d n. d n. d DnHP n. d n. d n. d BBP n. d n. d n. d DEHP n. d n. d DHP n. d n. d n. d DCHP n. d n. d n. d DnOP n. d n. d n. d DUP n. d n. d n. d n. d. The result was less than the LOD. - It is difficult to obtain accurate recovery because the content in the sample is too high.
7 PAE 4 19 PAEs 1. 0 μg /g Table 4 Contents of 19 PAEs in hair vaseline lotion and nail polish samples and recoveries of 19 PAEs spiked in 3 cosmetic samples at 1. 0 μg /g Hair vaseline Lotion Nail polish Original / DMP n. d n. d DEP n. d n. d n. d. DAP n. d n. d n. d. DPP n. d n. d n. d. DIBP DBP n. d BMPP n. d n. d n. d. DIPP n. d n. d n. d. DMEP n. d n. d n. d. PIPP n. d n. d n. d. DnPP n. d n. d n. d. BEEP n. d n. d n. d. DnHP n. d n. d n. d. BBP n. d n. d n. d. DEHP n. d DHP n. d n. d n. d. DCHP n. d n. d n. d. DnOP n. d n. d n. d. DUP n. d n. d n. d. n. d. The result was less than the LOD. - It is difficult to obtain accurate recovery because the content in the sample is too high. 3 GC-MS 19 PAEs - 19 PAEs 1 Staples C A Peterson D R Parkerton T F et al. Chemosphere Bai J R Teng J. Cosmetics Formulation and Application Examples. Beijing China Petrochemical Press Wang X Y Lin X T Ke H M et al. Journal of Environment and 5 20 Health. 15 Zhou X J Zhao Y Q Li W et al. China Surfactant Detergent & Cosmetics. 4 McKee R H Butala J H David R M et al. Reprod Toxicol Zheng H H Li J Wu D N et al. Chinese Journal of Analysis Laboratory Chen H M Wang C Wang X et al. Journal of Instrumental A- nalysis Jen J F Liu T C. J Chromatogr A Liu C Li L S Wang S W et al. Chinese Journal of Chromatography US EPA 8061A 10 Lin F Wen Y Y Hong X Y et al. Analytical Instrumentation Earls A O Axford I P Braybrook J H. J Chromatogr A / Zhang L F Huang Y R Shi S X et al. Chromatography Chinese Journal of. 13 Zeng F Chen L X Cui K Y et al. Chinese Journal of Analytical Chemistry Wang F Zhang X Q Lu J et al. Flavour Fragrance Cosmetics Liu X P Huang W Li C Y et al. Journal of Environment and Health Shen H Y Jiang H L Mao H L et al. J Sep Sci
phthalate esters PAEs) n=12 n=20 - GC-MS 13 PAEs 18.77~ ng/l DiBP DEP 2- PAEs PAEs PAEs PAEs DnBP (2011)
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