GO/HF-SPME-HPLC-MS/MS测定牛奶中7种糖皮质激素

Determination of 7 Glucocorticoids Residues in Milk by GO/HF-SPME-HPLC-MS/MS

将氧化石墨烯(GO)作为中空纤维固相微萃取的吸附剂,结合高效液相色谱-串联质谱法用于牛奶中的糖皮质激素的测定。考察影响提取效率的条件(样品量、样品溶液pH、萃取方式、萃取时间、离子强度、解析溶剂种类、解析溶剂体积、解析时间)。在优化条件下,7种糖皮质激素在1~100μg/L内线性关系良好,相关系数不低于0.99,检出限为0.04~0.09μg/kg,定量限为0.12~0.30μg/kg。基质加标(0.400,0.800和2.00μg/kg)回收率在72.9%~89.0%之间,相对标准偏差(RSD,n=6)为1.1%~9.5%。该方法操作简单、快速、成本低,适用于牛奶中7种糖皮质激素残留的快速检测。

A hollow fiber-based solid phase microextraction coupled with high performance liquid chromatography-tandem mass spectrometry method was developed for the determination of 7 kinds of glucocorticoids in milk,using graphene oxide as the adsorbent.Factors that influence the extraction efficiencies were optimized,including the sample amount,pH of supernatant,extracted methods,adsorption time,ionic strength,the selection and dosage of eluent,and elution time.Under the optimized condition,7 kinds of glucocorticoids showed great linearity in the range of 1-100μg/L,with correlation coefficients higher than 0.99.The limits of detection and quantification were 0.04-0.09μg/kg and 0.12-0.30μg/kg.The recovery values of glucocorticoids residues(0.400,0.800 and 2.00μg/kg,n=6)arranged from 72.9%-89.0%,with 1.1%-9.5%of relative standard deviations(RSD,n=6).The method was simple,fast,cheap,and was suitable for monitoring 7 glucocorticoids residues in milk.