液相色谱-串联质谱法测定化妆品中地索奈德-21-醋酸酯

建立了液相色谱-串联质谱法测定化妆品中糖皮质激素地索奈德-21-醋酸酯的方法。样品经甲醇超声提取,通过SPE小柱净化,利用Poroshell 120 SB C18(1.8μm,2.1×75 mm)色谱柱分离,以0.1%甲酸水溶液和0.1%甲酸乙腈溶液为流动相,梯度洗脱。在电喷雾离子源的正离子模式下采用多反应监测(MRM)模式采集数据并进行测定。在优化的条件下,地索奈德-21-醋酸酯在10~200μg/mL范围内线性关系良好,相关系数大于0.999。在0.1、0.5、2.0μg/g 3个浓度加标水平下,平均回收率为90.1%~94.9%,相对标准偏差为1.4%~2.8%,检出限(S/N=3)为0.03μg/g,定量限(S/N=10)为0.10μg/g。该方法准确可靠、快速灵敏,可用于化妆品中地索奈德-21-醋酸酯的测定。

Determination of Desonide-21-Acetate in Cosmetics by Liquid Chromatography-Tandem Mass Spectrometry

A liquid chromatography-tandem mass spectrometry (LC-MS/MS) method for determination of desonide-21-acetate in cosmetics was developed.The cosmetic sample was extracted with methanol by ultrasonic extraction.A Poroshell 120 SB C 18 (1.8 μ m,2.1 × 75 mm) column was used to separate target and impurities.0.1％ Formic acid aqueous solution and 0.1％ formic acid acetonitrile solution were used as mobile phase.Gradient elution program was used to separate and analyze.Electrospray ionization (ESI) mass spectrometry was performed in the positive mode using multiple reaction monitor (MRM) mode for the qualitative and quantitative analyses.Under optimized condition,the calibration curves were linear in the range of 10～200 μtg/mL,the correlation coefficient was over 0.999.The average recoveries at three spiked levels of 0.1,0.5,2.0μtg/g were between 90.4％ and 94.9％,with relative standard deviations of 1.4％～2.8％.The limits of detection (LODs,S/N=3) were 0.03 μtg/g and the limits of quantitation (LOQs,S/N=10) were 0.10μg/g.The method is accurate,fast and sensitive enough to meet the requirement for determination of desonide-21-acetate in cosmetics.