PRiME HLB固相萃取-高效液相色谱-串联质谱法测定化妆品中的双酚A

Determination of Bisphenol A Residues Incosmetics by PRiME HLB-HPLC-MS-MS

建立了PRiME HLB固相萃取-高效液相色谱-串联质谱测定水状、膏霜状和精油状化妆品中的双酚A残留量的方法。化妆品基质采用5%氨水乙腈溶液提取,使用PRiME HLB固相萃取柱净化后,以Waters ACQUITY UPLC BEH C18(100 mm×Φ2.0 mm, 1.7μm)为色谱柱,甲醇-0.1%氟化铵水溶液为流动相,梯度洗脱。电喷雾离子源负离子扫描模式,多反应监测(MRM)进行检测。结果表明,双酚A在本方法下响应较好,在2~50 ng/mL范围内线性良好,相关系数大于0.99,各基质的平均加标回收率为92.5%~101.2%,相对标准偏差小于3.2%。该方法前处理快捷简便,定量准确可靠,能很好地检测化妆品中双酚A的残留量。

[JP2]A method was established for the determination of bisphenol Aresidues in various kinds of cosmetics by performance liquid chromatography-tandem mass spectrometry(HPLC-MS/MS).The samples were ultrasonically extracted with 5%ammonium in acetonitrile hydroxide solution and purified using PRiME HLB.The target compound was separated on a Waters ACQUITY UPLC BEH C 18 column(∅2.1mm×100mm,1.7μm)by gradient elution using methanol and 0.1%ammonium fluoride solutionas mobile phases.The analysis was carried out using a negative electrospray ion source in the multiple reaction monitoring mode.Results showed that under the optimized test conditions the target compound had big responsivity.There was a good linear relationship for bisphenol A in the range of 2~50 ng·mL-1,and the linear correlation coefficients was above 0.99.The average recoveries of the lower limit of quantitation were between 92.5%and 101.2%,and the relative deviations were less than 3.2%.The method is convenient,accurate,and is suitable for the determination of bisphenol A residues in various kinds of cosmetics.[JP]