超临界色谱法同时测定化妆品中维生素A类衍生物和维生素D2,D3

Determination of vitamin a derivatives, vitamin D2 and D3 in cosmetics by supercritical fluid chromatography

采用超临界色谱法建立了同时测定化妆品中维生素A乙酸酯、维生素A丙酸酯、维生素A棕榈酸酯、维生素D2和D3的分析方法。水溶性化妆品和油溶性化妆品经不同比例的水-乙腈-正己烷溶剂体系按不同的添加顺序进行分散、提取后,采用Viridis BEH 2-EP色谱柱（250×4.6 mm,5μm）,以CO2为流动相,异丙醇-正己烷（1∶1）为改性剂,进行梯度洗脱分离,光电二极管矩阵检测器（SFC-PDA）检测,结合保留时间和光谱图定性,外标标准曲线法定量。实验结果表明,5种目标物质量浓度在1.0-60 mg/L范围内线性关系良好,相关系数为0.9992-0.9996;维生素A乙酸酯、维生素A丙酸酯、维生素A棕榈酸酯的定量下限（S/N=10）为4.0 mg/kg,维生素D2和D3的定量下限（S/N=10）为8.0 mg/kg。空白基质加标回收率为93.8%-110.1%,相对标准偏差（RSDs）小于13%。方法适用于各类化妆品中维生素A乙酸酯、维生素A丙酸酯、维生素A棕榈酸酯、维生素D2和D3的测定。

A method was established for the simultaneous determination of Vitamin A acetate, Vitamin A propionate, Vitamin A palmitate, Vitamin D2 and D3 in cosmetics by supercritical fluid chromatography （SFC） with a photodiode-array （PDA） detector. The water-soluble and oil-soluble samples were sequentially dispersed and extracted with water-acetonitrile-hexane solvent system. After concentrated, the extracts were analyzed by SFC-PDA on a Viridis BEH 2-EP column（250 ×4. 6 mm, 5 μm） with CO2 as the mobile phase and 2-propanol：hexane （ 1 ： 1 ） as modifier by gradient elution. These compouds were qualitatively confirmed by retention time and ultraviolet spectra, and quantified with the external standard method. The results showed that the linear correlation coefficients of five targets ranged from 0. 9992 to 0. 9996 within the linear range of 1.0 - 60 mg/L. The limits of quantification （LOQ, S/N = 10） were 4. 0 mg/kg for Vitamin A acetate, Vitamin A propionate, Vitamin A palmitate and 8.0 mg/kg for Vitamin D2, D3. The average recoveries were between 93.8 % and 110. 1% with RSDs （n =6） less than 13%. The method was simple, rapid, accurate, and suitable for the determination of Vitamin A acetate, Vitamin A propionate, Vitamin A palmitate, Vitamin D2 and D3 in different cosmetics.