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

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。

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

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 extraction 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 under multiple reaction monitoring(MRM) with electrospry ionization in negative ion mode(ESI-),identified 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 0.5-50.0 μg/L with correlation coefficients more than 0.999.The quantitation limits were 0.5 μg/kg.The mean recoveries for four compounds in skin water 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.