高效液相色谱-串联质谱法测定粉状化妆品中氟轻松

Determination of fluocinolone acetonide in powder cosmetics by high performance liquid chromatography-tandem mass spectrometry

目的为监测化妆品中的氟轻松含量以提供风险评估依据,本研究建立了粉状化妆品中氟轻松的高效液相色谱-串联质谱分析方法。方法样品经饱和氯化钠-乙酸乙酯提取后,过Oasis HLB固相萃取小柱净化,采用Waters BEH C18柱(2.1 mm×50 mm,1.7μm)分离,以0.1%乙酸-乙腈-0.1%乙酸水溶液为流动相梯度洗脱,MS/MS多反应监测模式检测。结果氟轻松在50 ng/ml^500 ng/ml时响应值与浓度呈良好线性关系,方法检出限为0.03μg/g,3种加标浓度下样品的加标回收率为82.4%~95.2%,相对标准偏差(RSD)为2.2%~4.6%。结论本方法通过对目标物的有效净化和富集,能有效除去基质干扰,提高方法灵敏度,降低基质效应,实现了快速测定,准确定量和确证的目的,适用于粉状化妆品中氟轻松的检测。

Objective In order to provide reference for the sampling inspection and risk assessment,in this study a method for determination of fluocinolone acetonide in powder cosmetics by high performance liquid chromatography-tandem mass spectrometry（ HPLC-MS/MS） was established. Methods The samples were extracted with saturated sodium chloride-ethyl acetate and then pre-purified by an Oasis HLB SPE cartridge. The pretreated samples were separated on a Waters BEH C18 column（ 2. 1 mm ×50 mm,1. 7 μm） by using 0. 1% acetic acid acetonitrile solution-0. 1% acetic acid aqueous solution as mobile phase. The analytes were detected by tandem mass spectrometer with electrospray ionization source in multiple reaction monitoring（ MRM）.Results Good linearity was obtained when the concentration of fluocinolone acetonide was within 50 ng/ml-500 ng/ml,with limits of determination of 0. 03 μg/g. The recovery rate was within 82. 4%-95. 2% at three spiked levels of different samples,with relative standard deviation（ RSD） of 2. 2%-4. 6%. Conclusion The method based on the effective purification and enrichment of the target can effectively eliminate matrix interference,improve sensitivity,reduce matrix effect,and achieve the purpose of rapid determination and accurate quantification. The method is suitable for the analysis of fluocinolone acetonide in powder cosmetics.