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建立了固相萃取-液相色谱-串联质谱法测定多种食用活动物猪、牛和羊的尿液及其血液,鸡的血液,鱼肉、虾肉、蛇肉和田螺肉中4种四环素类药物的分析方法。所测样品经0.1 mol/L Na2EDTA-Mcllvain缓冲溶液(p H 4.0(±0.5))提取后,以Oasis HLB固相萃取柱净化富集,在HPLC/MS/MS多反应监测(MRM)模式下进行了定性和定量分析。在上述检测条件下,所测的4种四环素类药物的最低检出限为1.00μg/kg,平均回收率为88.50%~96.70%,线性范围为1.00~100.00μg/L。
A method was developed for the determination of four kinds of tetracyclines in blood, fish, shrimp, snake and snail meat of a variety of edible live animals, such as pigs, cattle and sheep, by solid-phase extraction coupled with liquid chromatography-tandem mass spectrometry Drug analysis methods. The samples were extracted with 0.1 mol / L Na2EDTA-Mcllvain buffer solution (pH 4.0 (± 0.5)), and then were purified by Oasis HLB SPE cartridge. The HPLC-MS / MS multiple reaction monitoring A qualitative and quantitative analysis was conducted. Under the above conditions, the detection limits of four tetracyclines were 1.00μg / kg and the average recoveries were 88.50% ~ 96.70%. The linear range was 1.00-100.00μg / L.