超高效液相色谱-高分辨率质谱法筛查化妆品中12种糖皮质激素  

Screening of 12 Glucocorticoids in Cosmetics by High Performance Liquid Chromatography-High Resolution Mass Spectrometry

作　　者：李强[1,2] 张晓光[1,2] 马俊美[1,2] 李润岩[1,2] 范素芳[1,2] 张岩[1,2] 

机构地区：[1]河北省食品检验研究院,河北石家庄050091 [2]河北省食品安全重点实验室,河北石家庄050091

出　　处：《分析测试学报》2016年第2期179-184,共6页Journal of Instrumental Analysis

摘　　要：建立了超高效液相色谱-四极杆-静电场轨道阱质谱快速筛查和确证化妆品中可能添加的12种糖皮质激素的分析方法。样品经乙腈提取,用Acquity UPLC BEH C18柱(100 mm×2.1 mm,1.7μm)分离,以0.1%甲酸甲醇和0.1%甲酸水溶液为流动相进行梯度洗脱。以正离子全扫描模式得到糖皮质激素的精确质量数,与理论精确质量数对比,精确度偏差小于2×10-6。建立了筛查列表,并将12种糖皮质激素物质的二级质谱数据库加入确证条件中,实现了对12种糖皮质激素类物质的快速筛查。检出限为1~2μg/kg,定量下限为3~5μg/kg;加标水平为10,20,40μg/kg时,回收率为78.3%~112.5%,相对标准偏差(RSD)为1.0%~11.2%。该方法可作为化妆品中非法添加糖皮质激素成分的高通量筛选和确认检测方法。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（ 100 mm × 2. 1 mm,1. 7 μm） 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 1 μg / kg to 2 μg / kg,and the limits of quantitation（ LOQ） ranged from 3 μg / kg to 5 μg / kg. Satisfactory recoveries from 78. 3% to115. 2% were obtained at spiked concentration levels of 10,20,40 μg / 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 

分 类 号：O657.63[理学—分析化学] O629.8[理学—化学]