HPLC-MS/MS法测定3种不同基质化妆品中10种斯汀类禁用药物

Determination of 10 prohibited stines in 3 different matrixes of cosmetics by HPLC-MS/MS

建立了高效液相色谱-质谱联用法(HPLC-MS/MS)测定3种不同基质类型化妆品中10种斯汀类禁用药物的分析方法。样品经0.1%甲酸-乙腈超声提取后,采用Agilent Eclipse plus C_(8)(2.1 mm×100 mm,1.8μm)色谱柱,以甲醇-5 mmol/L甲酸铵0.1%甲酸水溶液作为流动相梯度洗脱。使用三重四极杆质谱多反应监测模式(MRM)检测,标准曲线外标法定量。结果表明,盐酸倍他司汀、咪唑斯汀、盐酸依匹斯汀、富马酸依美斯汀在1~16μg/L质量浓度范围,其余六种斯汀类在0.1~1.6μg/L质量浓度范围内线性良好,相关系数(r^(2))>0.99,检出限(LOD)和定量下限(LOQ)分别为0.003~0.12μg/L和0.011~0.39μg/L。3个不同质量浓度添加水平下,水剂、乳液类和膏霜类样品回收率分别为88.0%~107.8%,87.1%~106.5%和87.1%~107.7%,相对标准偏差(RSD)<10%。该方法前处理简单、高效、方法回收率高重复性好,适用于水剂、乳液和膏霜类化妆品中10种斯汀类禁用药物的同时测定。

A high performance liquid chromatography-tandem mass spectrometry(HPLC-MS/MS)method has been established for the simultaneous determination of 10 banned stines drugs in 3 different matrixes of cosmetics.The sample was ultrasonically extracted with 0.1%formic acid-acetonitrile and performed on an Agilent Eclipse plus C8 column(2.1 mm×100 mm,1.8μm)with gradient elution using methanol and 5 mmol/L ammonium formate-0.1%formic acid aqueous solution as the mobile phase.The determination was performed by MS/MS in multiple reaction detection(MRM)mode,and the external standard method was used for quantification.Betahistine dihydrochlorride,mizolastine,epinastine hydrochloride,and emedastine difumarate have good linearity in the range of 1-16μg/L,while the other six stines have good linearity in the range of 0.1-1.6μg/L,with the correlation coefficient(r2)>0.99.The limits of detection(LODs)and the limits of quantification(LOQs)are in the range of 0.003-0.12μg/L and 0.011-0.39μg/L,respectively.At three different levels of addition,the recoveries of water aqua,lotion and cream samples are 88.0%-107.8%,87.1%-106.5%,and 87.1%-107.7%,respectively.And the relative standard deviation(RSD)is less than 10%.The method is accurate,high-efficiency,simple pre-treatment,and high recovery rate.It is suitable for the simultaneous determination of 10 stines in cosmetics.