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

摘要

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 C18 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 min. The calibration curves for four compounds were linear in the range of 0. 5 - 50. 0μg/L with correlation coefficients more than 0. 999. The quantitation limits were 0. 5μg/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.%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,氧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0.5-50.0 μg/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、10.0 μg/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.