【摘要】 采用液相色谱-串联质谱在多反应监测模式下测定蜂王浆中7种糖皮质激素残留。试样中加入p H 5.2的乙酸铵缓冲盐溶液和β-葡萄糖醛酸甙酶/芳基硫酸酯酶,37℃恒温箱中放置16 h。甲醇超声提取,去除部分蛋白质,依次经HLB柱和氨基柱净化,液相色谱-串联质谱仪检测。该方法在0~80μg/kg范围内具有良好的线性关系。实验中添加水平为10、20和40μg/kg时,回收率范围为84.7%~100%;相对标准偏差小于9.9%;方法检出限(LOQ)均为10μg/kg。更多还原

【Abstract】 A method was developed for the determination of seven glucocorticoids residues in royal jelly by high performance liquid chromatography coupled with tandem mass spectrometry. The samples were hydrolyzed with the ammonium acetate(p H 5.2) buffer solution and β-glucuronidase/arylsulfatase, 37 ℃ thermostat for 16 h. Some proteins were removed by ultrasonic extraction of methanol and purified by HLB solid phase extraction column and amino column, and detected by high performance liquid chromatography coupled with tandem mass spectrometry. The method showed good linearities in the range of 0 ~ 80 μg/kg. In the experiment, spiked at the levels of 10, 20 and 40 μg/kg, the spiked recoveries ranged from 84.7% to 100% with relative standard deviations was less than 9.9%, the limits of quantification(LOQ) was 10 μg/kg.更多还原