超高效液相色谱-串联质谱法测定化妆品中新型糖皮质激素氯倍他索乙酸酯  

Determination of new glucocorticoid called clobetasol acetate in cosmetics by ultra performance liquid chromatography-tandem mass spectrometry

作　　者：杨飘飘 黄伟 李丽霞 刘红 YANG Piaopiao;HUANG Wei;LI Lixia;LIU Hong(Hubei Institute for Drug Control,Hubei Engineering Research Center for Drug Quality Control,Wuhan 430075,China)

机构地区：[1]湖北省药品监督检验研究院,湖北省药品质量检测与控制工程技术研究中心,湖北武汉430075

出　　处：《色谱》2023年第3期250-256,I0002,共8页Chinese Journal of Chromatography

基　　金：湖北省药品监督管理局2020~2021药品监管科研项目(20200203)。

摘　　要：采用超高效液相色谱-串联质谱法建立了化妆品中氯倍他索乙酸酯的检测方法,适用于膏霜乳类、凝胶类、泥类、贴膜类和液体(水)类5种常见化妆品基质。对影响被测物质的前处理方法、提取溶剂、提取时间等因素和色谱、质谱条件等进行了考察。最终建立方法为样品经乙腈涡旋分散、超声提取、过滤后用超高效液相色谱-串联质谱仪测定,采用Waters CORTECS C_(18)色谱柱(150 mm×2.1 mm,2.7μm),以水和乙腈作为流动相分离,在电喷雾正离子模式(ESI+)下,以多反应监测(MRM)方式采集,采用基质匹配标准曲线进行定量分析。5种基质类型下,被测物质在0.9~37μg/L的范围内线性拟合良好,线性相关系数(R^(2))均超过0.99。方法的检出限为0.03μg/g,定量限为0.09μg/g。在定量限、2倍定量限和10倍定量限3个水平下的加标回收率试验中,被测物质在5种基质中的回收率范围为83.2%~103.2%,相对标准偏差(RSD,n=6)范围为1.4%~5.6%。采用该方法对不同基质类型的化妆品样品进行筛查,共发现5批阳性样品,其中氯倍他索乙酸酯的含量范围为1.1~48.1μg/g。该方法操作简单,灵敏可靠,适用于不同基质类型化妆品的高通量定性定量筛查分析,为监测化妆品中的非法添加提供了技术支持及理论依据。At present,new prohibited substances are becoming more common illegal additions in cosmetics.Clobetasol acetate is a new glucocorticoid,which is not covered in the current national standards and is a homologue of clobetasol propionate.A method was established for the determination of clobetasol acetate as a new glucocorticoid(GC)in cosmetics by ultra performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS).Five common cosmetic matrices were suitable for this new method:creams,gels,clay masks,masks and lotions.Four pretreatment methods were compared:direct extraction by acetonitrile,PRiME pass-through column purification,solid-phase extraction(SPE)purification,and QuEChERS purification.Further,the effects of different extraction efficiencies of the target compound,such as extraction solvents and extraction time,were investigated.The MS parameters,such as ion mode,cone voltage and collision energy of ion pairs of the target compound,were optimized.The chromatographic separation conditions and response intensities of the target compound in different mobile phases were compared.Based on the experimental results,the optimal extraction method was determined to be direct extraction,wherein the samples were vortex dispersed with acetonitrile,ultrasonic extraction over 30 min and filtered by a 0.22μm organic millipore filter,and then the samples were detected by UPLC-MS/MS.The concentrated extracts were separated on a Waters CORTECS C_(18)column(150 mm×2.1 mm,2.7μm),where the water and acetonitrile were used as the mobile phases for gradient elution.The target compound was detected with the multiple reaction monitoring(MRM)mode under electrospray ionization and positive ion scanning(ESI+).Quantitative analysis was performed by matrix matching standard curve.Under the optimum conditions,the target compound had good linear fitting in the range of 0.9-37μg/L.The linear correlation coefficient(R^(2))was greater than 0.99,the limit of quantification(LOQ)of the method was 0.09μg/g and the limit of detection(L

关 键 词：超高效液相色谱-串联质谱 糖皮质激素 氯倍他索乙酸酯 化妆品 

分 类 号：O658[理学—分析化学]