色谱2017，Vol.35Issue(8)：816-825,10.DOI:10.3724/SP.J.1123.2017.04005
分散固相萃取-液相色谱-串联质谱法同时快速测定化妆品中81种糖皮质激素
Simultaneous rapid determination of 81 glucocorticoids in cosmetics by dispersive solid phase extraction and liquid chromatography-tandem mass spectrometry
摘要
Abstract
A novel method was developed for the simultaneous rapid determination of 81 illegally added glucocorticoids (GCs) in cosmetics using dispersive-solid phase extraction (d-SPE) and liquid chromatography-tandem mass spectrometry (LC-MS/MS).The analytes were extracted by acetonitrile after dispersing with water, and then purified using the C18 and primary secondary amine (PSA).The chromatographic separations were performed on a Poroshell 120 PFP column (100 mm×2.1 mm, 2.7 μm) under multiple chromatographic retention modes.Acetonitrile and 0.2% (v/v) acetic acid aqueous solution were used as mobile phases with gradient elution, and all the 10 groups of isomers were baseline separated.The qualitative identification and quantitative analysis of the 81 GCs were operated in the electrospray ionization positive mode using dynamic multiple reaction monitoring (DMRM).The 81 GCs finally were quantified by internal standard method.The correlation coefficients of linear calibration curves were greater than 0.99 in the corresponding mass concentration ranges.The average recoveries of the 81 GCs at three spiked levels ranged from 68.8% to 105.3% with relative standard deviations (RSDs) of 2.9%-13.1% (n=6).The LODs (S/N≥3) and LOQs (S/N≥10) were 0.002-0.006 μg/g and 0.005-0.020 μg/g, respectively.A number of 137 cosmetic samples submitted by customers were screened.Sixteen positive samples were found, and the contents of GCs were from 16.9 μg/g to 158 μg/g.The results showed that the new method is simple, rapid, sensitive and reliable, and it is suitable for qualitative and quantitative screening analysis of the 81 GCs in cosmetics simultaneously.关键词
液相色谱-串联质谱/分散固相萃取/同位素稀释/非法添加/糖皮质激素/化妆品Key words
liquid chromatography-tandem mass spectrometry (LC-MS/MS)/dispersive-solid phase extraction (d-SPE)/isotope dilution/illegally added/glucocorticoids (GCs)/cosmetics分类
化学化工引用本文复制引用
罗辉泰,黄晓兰,吴惠勤,张秋炎,朱志鑫,黄芳,林晓珊,马叶芬,邓欣..分散固相萃取-液相色谱-串联质谱法同时快速测定化妆品中81种糖皮质激素[J].色谱,2017,35(8):816-825,10.基金项目
广东省省级科技计划项目(2014A040401038,2014B070705001).Science and Technology Plan Project of Guangdong Province of China (Nos.2014A040401038, 2014B070705001). （2014A040401038,2014B070705001）
