建立了化妆品中丙烯酰胺残留的同位素稀释液相色谱-串联质谱的分析方法.水溶性化妆品样品以水为提取溶剂进行提取,提取液经高速离心处理后,上清液用Oasis HLB固相萃取柱净化;脂溶性化妆品样品以正己烷和水混合溶剂液-液分配萃取.经Waters Atlantis T3色谱柱(150 mm×2.1 mm,3 μm)分离后在多反应监测模式下进行串联质谱定性及定量分析,以~(13)C_3-丙烯酰胺为内标定量.方法的定量限为0.1 mg/kg,在0.1～1.0 mg/kg 3个添加水平范围内的平均回收率为87.7% ～95.8%,日内测定精密度均小于10%,日间测定精密度均小于12% .该方法能够满足化妆品中丙烯酰胺残留的检测要求.
A comprehensive analytical method based on isotope dilution-liquid chromatography-tandem mass spectrometry (LC-MS/MS) has been developed for the determination of acrylam-ide residue in cosmetics. Water-soluble cosmetic sample was extracted with water, and the ex-tract was centrifuged, then the upper solution was cleaned up by an Oasis HLB solid phase ex-traction cartridge. Oil-soluble cosmetic sample was extracted by liquid-liquid partition with n-hexane and water. The qualitative and quantitative analyses were carried out for the analyte in the multiple reaction monitoring (MRM) mode after the chromatographic separation on a Wa-ters Atlantis T3 column (150 mm × 2. 1 mm, 3 μm). The quantification was performed with ~(13)C_3-acrylamide as internal standard. The limit of quantification (LOQ) for acrylamide was 0. 1 mg/kg. The mean recoveries were 87. 7% -95. 8% at the spiked levels of 0.1-1.0 mg/kg with the intra-day precision less than 10% and the inter-day precision less than 12%. The method is suitable for the determination of acrylamide in cosmetics.
参考文献
| [1] | Pepe R C,Wenninger J A,McEwen G N Jr.International cosmetic ingredient dictionary and handbook.9th ed.Vol 2.Washington,DC:CTFA,2002 |
| [2] | Taylor D E,Penhallow J E.Biomaterials,1986,7(4):277 |
| [3] | Wu Y N,Jiang G B.Trace and ultra-trace inspection technology of important organic pollutants.Beijing:Chemical Industry Press (吴永宁,江桂斌.重要有机污染物痕量与超痕量检测技术.北京:化学工业出版社),2007 |
| [4] | Ministry of Health of China.Hygienic standard for cosmetics.Beijing:Ministry of Health of the People's Republic of China (卫生部.化妆品卫生规范.北京:中华人民共和国卫生部),2007 |
| [5] | 76/768/EEC.(2006-12-10).http:/ /europa.eu.int/eur-lex/en/consleg/main/1976/en_1976L0768_index.html |
| [6] | Cosmetic Ingredient Review:Quick Reference Table.[2009-02-15].http:/ /www.cir-safety.org/staff_files/ReferenceTable.pdf |
| [7] | Barber D S,Hunt J,LoPachin R M,et al.J Chromatogr B,2001,758(2):289 |
| [8] | Zhang Y,Dong Y,Ren Y P,et al.J Chromatogr A,2006,1 116(1/2):209 |
| [9] | Tezcan F,Erim B.Anal Chim Acta,2008,617(1/2):196 |
| [10] | Geng Z M,Jiang R,Chen M.J Food Compost Anal,2008,21(2):178 |
| [11] | Liu J,Zhao G H,Yuan Y,et al.Food Chemistry,2008,108(2):760 |
| [12] | Zhang Y,Jiao J J,Cai Z X,et al.J Chromatogr A,2007,1 142(2):194 |
| [13] | Hoenicke K,Gatermann R,Harder W,et al.Anal Chim Acta,2004,520(1/2):207 |
| [14] | Skelly N E,Husser E R.Anal Chem,1978,50(14):1 959 |
| [15] | 2002/657/EC.[2002-08-12].http:/ /eur-lex.europa.eu/pri/en/oj/dat/2002/l_221/l_22120020817en00080036.pdf |
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