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Simultaneous Determination of Twelve Glucocorticoids Residues in Milk by Ultra Performance Liquid Chromatography-Electrospray Tandem Mass Spectrometry
Author(s): 
Pages: 213-217
Year: Issue:  3
Journal: CHINESE JOURNAL OF CHROMATOGRAPHY

Keyword:  超高效液相色谱-串联质谱法固相萃取糖皮质激素残留牛奶;
Abstract: 采用超高效液相色谱-串联电喷雾四极杆质谱(负离子模式)在多反应监测(MRM)模式下测定了牛奶中12种糖皮质激素的残留.试样中加入pH 5.20的醋酸盐缓冲溶液和甲醇,超声提取,以去除部分蛋白质,然后用正己烷脱脂,依次经HLB柱、硅胶柱和氨基柱等固相萃取柱浓缩和净化后,通过Waters ACQUITY UPLCTM BEH C18色谱柱分离,以甲醇和含0.1%甲酸的水为流动相进行梯度洗脱.在超高效液相色谱-质谱分析过程中以保留时间和离子对(母离子和两个碎片离子)信息比较进行定性,以母离子和响应值高的碎片离子进行定量.该法的检出限为0.02~0.38 μg/kg,最低定量限为0.07~1.27 μg/kg.添加水平为2 μg/kg和0.4 μg/kg时,12种糖皮质激素的加标回收率为69.3% ~94.3% ,相对标准偏差为3.5% ~16.7% .
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