超高效液相色谱-串联质谱法同时测定化妆品中7种双酚类化合物及其衍生物

Simultaneous determination of seven bisphenols and bisphenol derivatives in cosmetics by ultra performance liquid chromatography-tandem mass spectrometry

建立同时快速测定化妆品中7种双酚类化合物及其衍生物的超高效液相色谱-串联质谱方法。水剂化妆品采用正己烷-乙酸乙酯(体积比为1∶1)溶液超声提取;粉类、膏霜乳液类、凝胶类化妆品采用乙酸乙酯超声提取,提取液经氮吹浓缩后用甲醇-水(体积比为1∶1)溶液定容,用Waters XSelect HSS T3(100 mm×2.1μm,1.7μm)色谱柱分离,采用质谱多反应监测模式检测,色谱峰面积外标法定量。7种双酚类化合物及其衍生物的质量浓度在0.1~50.0 ng/mL范围内与色谱峰面积线性关系良好,相关系数均不小于0.996,检出限为0.1 ng/mL。在样品基质中分别添加0.1,0.5,2.0μg/kg 3种浓度水平的混合标准溶液进行加标回收试验,7种双酚类化合物及其衍生物的加标回收率为84.5%~119.2%,测定结果的相对标准偏差为1.19%~4.92%(n=6)。该方法可用于化妆品中7种双酚类化合物及其衍生物的定性和定量分析。

An ultra high performance liquid chromatography-tandem mass spectrometry method for the simultaneous and rapid determination of seven bisphenol compounds and their derivatives in cosmetics was established. Aqueous cosmetics were ultrasonically extracted with n-hexane-ethyl acetate(volume ratio was 1∶1);powders, creams, emulsions,and gel cosmetics were ultrasonically extracted with ethyl acetate. The extract was concentrated by nitrogen blowing and then fixed to volume with methanol water(volume ratio was 1∶1);separated by Waters XSelect HSS T3(100 mm×2.1μm,1.7 μm) chromatographic column, detected by mass spectrometry multi-reaction monitoring mode, and quantified by external standard method of chromatographic peak area. The mass concentration of 7 bisphenol compounds and their derivatives had a good linear relationship with the chromatographic peak area in the range of 0.1-50.0 ng/mL, the correlation coefficients were not less than 0.996, and the detection limit was 0.1 ng/mL. Three levels of 0.1, 0.5, 2.0 μg/kg mixed standard solutions were added to the sample matrix to perform the spike recovery test, the spike recoveries of 7 bisphenol compounds and their derivatives were 84.5%-119.2%, and the relative standard deviation of the determination results was 1.19%-4.92%(n=6). This method can be applied to the qualitative and quantitative analysis of seven bisphenol compounds and their derivatives in cosmetics.