化妆品中1-羟乙基-4,5-二氨基吡唑硫酸盐等3种染发剂的高效液相色谱法测定及质谱确证

Determination of Three Hair Dyes in Cosmetics by High Performance Liquid Chromatography and Confirmation by Liquid Chromatography Tandem Mass Spectrometry

建立了以高效液相色谱法(HPLC)测定化妆品中3种染发剂(1-羟乙基-4,5-二氨基吡唑硫酸盐、2-氨基-6-氯-4-硝基苯酚、5-氨基-6-氯-2-甲基苯酚)的分析方法。样品采用体积分数50%乙醇(含1 g/L亚硫酸氢钠)冰浴超声提取,经ZORBAX Eclipse Plus Phenyl-Hexyl(250 mm×4.6 mm×5μm)色谱柱分离后,用二极管阵列检测器(DAD)进行检测。以保留时间和紫外吸收光谱定性,外标法定量,液相色谱-串联质谱法(LC-MS/MS)确证。结果表明:3种染发剂的方法检出限(LOD)和定量限(LOQ)分别为24~53μg/g和80~175μg/g,在各自范围线性关系良好,相关系数(r)>0.999,平均回收率为81.9%~103.9%,相对标准偏差(RSD)为0.1%~2.5%(n=6)。该方法快速、高效、准确,适用于化妆品中1-羟乙基-4,5-二氨基吡唑硫酸盐等3种染发剂的测定。

A high performance liquid chromatographic(HPLC)method was established for the determination of 3 hair dyes in cosmetics,including 4,5-diamino-1-(2-hydroxyethyl)pyrazole sulfate,2-amino-6-chloro-4-nitrophenol,5-amino-6-chloro-2-methylphenol.The samples were extracted with 50%(volume fraction)ethanol(containing 1 g/L NaHSO3),then separated on a ZORBAX Eclipse Plus Phenyl-Hexyl(250 mm×4.6 mm×5μm)column and detected by DAD.The qualitative analyses were based on retention time and ultraviolet absorbance,while quantitative analyses were performed by the external standard method.The positive samples were confi rmed by LC-MS/MS.The limit of detection(LOD)and limit of quantitation(LOQ)were 24-53μg/g and 80-175μg/g,respectively.The calibration curves showed good linearity with correlation coeffi cients more than 0.999.The average recoveries were in the range of 81.9%and 103.9%with RSDs of 0.1%to 2.5%(n=6).The method is fast,effi cient,accurate,and could be applied for the determination of 3 hair dyes in cosmetics.