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OA北大核心CSTPCD

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.