Captiva EMR固相萃取-高效液相色谱-串联质谱法测定化妆品中41种糖皮质激素的含量  

Determination of 41 Glucocorticoids in Cosmetics by Captiva EMR Solid Phase Extraction-High Performance Liquid Chromatography-Tandem Mass Spectrometry

作　　者：温家欣[1] 黄钰萍 何嘉雯 刘亚雄[1] 陈俏[1] 赖宇红[1] WEN Jiaxin;HUANG Yuping;HE Jiawen;LIU Yaxiong;CHEN Qiao;LAI Yuhong(Guangdong Institute for Drug Controls Guangzhou 510663,China)

机构地区：[1]广东省药品检验所,广州510663

出　　处：《理化检验（化学分册）》2022年第2期140-147,共8页Physical Testing and Chemical Analysis(Part B:Chemical Analysis)

基　　金：广东省医学科学技术研究基金(B2020196);国家药品监督管理局药品快速检验技术重点实验室(国药监科外函[2019]82号-24)。

摘　　要：提出了Captiva EMR固相萃取结合高效液相色谱-串联质谱法(HPLC-MS/MS)同时测定化妆品中41种糖皮质激素含量的方法。样品经水分散后,用含1%(体积分数)甲酸的乙腈溶液提取目标化合物,以Captiva EMR固相萃取柱去除化妆品基质中的长链烃类化合物。在用HPLC分析时,采用Thermo Accoure PFP色谱柱(100 mm×2.1 mm,2.6μm)为固定相,含0.1%(体积分数,下同)乙酸的乙腈溶液-0.1%乙酸溶液的混合溶液作为流动相进行梯度洗脱;在MS/MS分析时,以电喷雾离子源正离子(ESI^(+))模式和多反应监测(MRM)模式进行检测,外标法定量。结果显示:在优化的试验条件下,目标化合物中较难分离的6组同分异构体均能得到有效分离,膏霜、乳液、洗面奶、凝胶、面膜的基质效应对大多数目标化合物的影响较弱;41种目标化合物标准曲线的线性范围均为1.5~100μg·L^(-1),相关系数为0.9934~1.000,检出限(3S/N)为0.015~0.05 mg·kg^(-1);以阴性膏霜、乳液、洗面奶、凝胶、面膜为基质进行加标回收试验,所得回收率为57.8%~121%,测定值的相对标准偏差(n=6)为0.50%~15%。方法用于60批化妆品的分析,检出2批阳性样品,检出量分别为32.3 mg·kg^(-1)(氯倍他索丙酸酯)和1.8 mg·kg^(-1)(地塞米松)。A method was established for the simultaneous determination of 41 glucocorticoids in cosmetics by Captiva EMR solid phase extraction combined with high performance liquid chromatography-tandem mass spectrometry(HPLC-MS/MS).After the sample was dispersed by water,the target compounds were extracted with acetonitrile solution containing 1%(volume fraction)formic acid and Captiva EMR solid phase extraction column was used to remove long-chain hydrocarbons from the cosmetic matrix.In HPLC analysis,Thermo Accoure PFP chromatographic column was used as stationary phase,and mixed solution composed of acetonitrile solution containing 0.1%(volume fraction,the same below)acetic acid and 0.1% acetic acid solution was used as mobile phase for gradient elution.In MS/MS analysis,ESI^(+) mode and MRM mode were used for detection,and external standard method was used for quantification.It was shown that under the optimized test conditions,the six groups of isomers which were difficult to be separated in the target compounds could be separated effectively,and the matrix effect of cream,lotion,facial cleanser,gel and mask had a weak effect on most of the target compounds.Linear ranges of standard curves for 41 compounds found were all 1.5-100μg·L^(-1),with correlation coefficients of 0.9934-1.000 and detection limits(3 S/N)of 0.015-0.05 mg·kg^(-1).The spiked recovery test was made on five matrices of cream,lotion,facial cleanser,gel and mask,giving recoveries in the range of 57.8%-121%,and RSDs(n=6)of determined values in the range of 0.50%-15%.The proposed method was applied for the analysis of the 60 batches of cosmetics,and 2 batches of positive samples were detected,with detection amount of 32.3 mg·kg^(-1) for clobetasol propionate and 1.8 mg·kg;for dexamethasone.

关 键 词：Captiva EMR固相萃取 高效液相色谱-串联质谱法 糖皮质激素 化妆品 

分 类 号：O657.63[理学—分析化学]