液相色谱串联质谱法测定化妆品中的双酚A、辛基酚及壬基酚  

Simultaneous Determination of Bisphenol A,Octylphenol and Nonylphenol in Skin Care Cosmetics by Liquid Chromatography-Tandem Mass Spectrometry

作　　者：郭新东[1] 冼燕萍[1] 陈立伟[1] 吴文海[1] 罗海英[1] 吴玉銮[1] 

机构地区：[1]广州市质量监督检测研究院国家化妆品质量监督检验中心(广州),广东广州510110

出　　处：《分析测试学报》2012年第7期848-852,共5页Journal of Instrumental Analysis

基　　金：国家质检总局科技计划项目(2009QK325)

摘　　要：建立了护肤化妆品中双酚A、辛基酚和壬基酚的超高效液相色谱串联质谱分析方法。样品经二氯甲烷提取,氨基固相萃取柱净化后,用甲醇定容,采用Waters UPLC BEH C18色谱柱,以甲醇-0.05%氨水为流动相,梯度洗脱分离后,串联四极杆质谱多反应监测方式检测,以保留时间和子离子比定性,外标法定量。在优化条件下,该方法 5 min内可完成4种待测物的分析。双酚A、辛基酚和壬基酚在0.5～50.0μg/L范围内线性关系良好,相关系数均大于0.999,方法的定量下限(LOQs)均为0.5μg/kg;在加标水平为0.5、1.0、10.0μg/kg时,护肤霜和护肤水样品中4种待测物的平均加标回收率为80%～96%,相对标准偏差(n=6)小于15%。该方法准确、快速、灵敏,适用于护肤化妆品中双酚A、辛基酚和壬基酚的快速确认和定量检测。A comprehensive analytical method for the determination of bisphenol A, octylphenol and nonylphenol in skin care cosmetics was developed using ultra performance liquid chromatography with tandem mass spectrometry（ UPLC -MS/MS）. The homogenized sample was extracted with methylene chloride. Sample concentration and purification were performed on an OASIS NH2 solid phase extrac- tion cartridge. The separation of 4 compounds was carried out on a Waters UPLC BEH Cls column by gradient elution with methanol- 0. 5% NH3 · H2O as mobile phase. The analytes were detected un- der multiple reaction monitoring（MRM） with electrospry ionization in negative ion mode（ESI-）, i- dentified with retention time and ion ratio, and quantified by the external standard method. Under the optimal conditions, the separation of analytes was performed within 5 rain. The calibration curves for four compounds were linear in the range of 0. 5 -50.0 I^g/L with correlation coefficients more than 0. 999. The quantitation limits were 0.5 μg/kg. The mean recoveries for four compounds in skin wa- ter and skin cream samples at three spiked concentration levels of 0. 5, 1.0, 10. 0 μg/kg were in the range of 80% -96% with RSDs（n = 6） less than 15%. This method is accurate, simple and rapid, and is suitable for the inspection of bisphenol A, octylphenol and nonylphenol in skin care cosmetics.

关 键 词：护肤化妆品 固相萃取 液相色谱串联质谱法 双酚A 辛基酚 壬基酚 

分 类 号：O657.7[理学—分析化学] O625.311[理学—化学]