超临界色谱法测定化妆品中生育酚及α-生育酚乙酸酯

Determination of Tocopherols and α-Tocopheryl Acetate in Cosmetics by Supercritical Fluid Chromatography

建立了化妆品中4种生育酚异构体及α-生育酚乙酸酯的超临界色谱分析方法.不同基质类型的化妆品经乙腈水溶液-正己烷溶剂体系按不同的添加顺序进行分散、提取、液液分配后,以二氧化碳为流动相,异丙醇-正己烷（1∶1）为改性剂,利用亚乙基桥杂化颗粒色谱柱（Viridis@BEH,250 mm＆#215;4.6 mm,5μm）对目标物和样品杂质进行有效分离,用光电二极管矩阵检测器（SFC-PDA）进行测定.系统考察了提取条件和色谱条件对实验结果的影响.结果表明：4种生育酚和α-生育酚乙酸酯的定量下限（S/N=10）分别为50 mg/kg和25 mg/kg,空白基质加标回收率为81.3％～ 109.5％,相对标准偏差（RSD）不大于12.8％.该方法前处理简单、快速、准确,可用于各类化妆品中4种生育酚异构体及α-生育酚乙酸酯含量的检测.

A supercritical fluid chromatographic （SFC） method was developed for the determination of tocopherols and α-tocopheryl acetate in cosmetics. Different types of samples were sequentialy dis- persed and extracted with acetonitrile water solution -hexane based on matix types. The chromato- graphic separation was conducted with a XBridge（ ViridisβEH, 250 mm x4.6 mm, 5 μm） by gra- dient elution using CO2 as mobile phase and 2-propanol ： hexane（ 1 ： 1 ） as modifier. The detection was performed with a photodiode - array （PDA） detector. The extraction procedures and chromato- graphic conditions were optimized. The results showed that the limits of quantitation （ LOQ, SIN = 10） were 50 mg/kg for four tocopherols and 25 mg/kg for α-tocopheryl acetate. The average recover- ies ranged from 81.3% to 109. 5% with relative standard deviations（RSDs） not more than 12.8% . The method is simple, rapid and accurate, and is suitable for the determination of four toeopherols and α-tocopheryl acetate in cosmetics.