A method was developed for screening of 12 kinds of glucocorticoids in cosmetics by high performance liquid chromatography-quadrupole/orbitrap high-resolution mass spectrometry(Orbitrap MS).The samples were extracted with acetonitrile,and separated with an Acquity UPLC BEH C18(100mm×2.1mm,1.7μm) using a binary solvent system composed of 0.1% formic acid methanol solution and 0.1% formic acid water solution by gradient elution.Accurate mass number of target compound were got in full scan mode.Compared to accurate mass number in theory,the mass accuracy error was below 2×10-6.The screening list was built,and the database of secondory characteristic fragment ions for the glucocorticoids were added in screening option.Qualitative screen was achieved.The limits of detection(LOD) of the method ranged from 1μg/kg to 2μg/kg,and the limits of quantitation(LOQ) ranged from 3μg/kg to 5μg/kg.Satisfactory recoveries from 78.3% to 115.2% were obtained at spiked concentration levels of 10,20,40μg/kg,and the relative standard deviations(RSDs) were in the range of 1.0%-11.2%.The method could be used for the determination of glucocorticoid in cosmetics as a high-throughput and confirmatory method.
关键词
超高效液相色谱四极杆-静电场轨道阱高分辨质谱糖皮质激素化妆品
Keywords
ultra high performance liquid chromatographyorbitrap mass spectrometry(Orbitrap MS)glucocorticoidcosmetic