分析测试学报2024，Vol.43Issue(7)：978-986,9.DOI:10.12452/j.fxcsxb.24040601
超高效液相色谱-串联质谱法测定膏霜乳类化妆品中法定标准以外的48种糖皮质激素
Determination of 48 Glucocorticoids Beyond Statutory Standard Methods in Cream-based Cosmetics by Ultra High Performance Liq-uid Chromatography-Tandem Mass Spectrometry
沈丹丹 1宫珊珊 1李悦忱 1薛恒跃 1于本涛 1姜博海 1王冬 1张蓉 2毛希琴1
作者信息
- 1. 大连市药品检验检测院,辽宁 大连 116021
- 2. 大连理工大学 化工学院,辽宁 大连 116024
- 折叠
摘要
Abstract
Current domestic statutory inspection methods for glucocorticoids in cosmetics included GB/T 24800.2-2009,GB/T 40145-2021 and the Safety and Technical Specification for Cosmetics(2015 edition),which covered 58 glucocorticoids in total.A method was developed to determine 48 glucocorticoids beyond statutory inspection methods in cream-based cosmetics by ultra high perfor-mance liquid chromatography-tandem mass spectrometry.After extraction and purification,samples were loaded on a Waters ACQUITY UPLC BEH C18 column(3.0 mm×150 mm,1.7 μm),where aqueous solution containing 0.2％acetic acid and methanol solution containing 0.2％acetic acid were used as mobile phases for gradient elution.After separation of target compounds,an electrospray ion-ization source in positive mode was used for mass analysis.All target compounds were analyzed with multiple reaction monitoring mode(MRM)and quantified by external standard method.The limits of detection(LODs,S/N≥3)and the limits of quantification(LOQs,S/N≥10)of the method for all tar-get compounds were 0.03 μg/g and 0.1 μg/g.The correlation coefficients(r)of 48 glucocorticoids were greater than 0.995 in the range of 2.5-60 μg/L.The matrix effects(MEs)of 48 kinds of glyco-corticoids in cream-based cosmetics were investigated via the addition of standard compounds to the extracted matrix solutions to make matrix standard curves.The MEs of all target compounds were with-in±15％,meaning that matrix effects are not significant.The average recoveries were 80.9％-1 10％with relative standard deviations(RSDs,n=6)of 0.70％-9.3％under spiked levels of 1,2 and 8 times of LOQ.One positive sample was confirmed through multiple reaction monitoring(MRM)-infor-mation dependent acquisition automated(IDA)-enhance product ion(EPI)to contain 0.3 μg/g of 6β-hydroxy triamcinolone acetonide.In conclusion,pre-processing method developed in this paper is simple and feasible and measurement results for 48 glucocorticoids are accurate and reliable,which can fill the regulatory gap of illegal addition of glucocorticoids in cosmetics.关键词
超高效液相色谱-串联质谱/糖皮质激素/化妆品/非法添加Key words
ultra high performance liquid chromatography-tandem mass spectrometry/glucocorti-coid/cosmetic/illegally added分类
化学引用本文复制引用
沈丹丹,宫珊珊,李悦忱,薛恒跃,于本涛,姜博海,王冬,张蓉,毛希琴..超高效液相色谱-串联质谱法测定膏霜乳类化妆品中法定标准以外的48种糖皮质激素[J].分析测试学报,2024,43(7):978-986,9.
