高效液相色谱-串联质谱法测定鱼肠道内容物中32种抗生素残留

Determination of 32 kinds of antibiotic residues in fish intestinal content by high performance liquid chromatography-tandem mass spectrometry

目的 建立高效液相色谱-串联质谱法测定鱼肠道内容物中32种抗生素残留的分析方法。方法 采用ACQUITY UPLC BEH C_(18)(2.1 mm×100 mm, 1.7μm)为分析色谱柱,乙腈及酸化乙腈为提取溶剂,通过兽药残留快速柱净化,以高效液相色谱-串联质谱仪测定,基质标准曲线定量。结果 该方法测定的32种抗生素检出限(limits of detection, LODs)为0.2-0.5μg/kg,定量限(limits of quantitation, LOQs)为1.0-1.5μg/kg;相对标准偏差(relative standard deviations, RSDs)为1.2%-12.8%, 3个加标浓度的回收率范围为79.5%-106.6%。在此基础上利用该方法分别对5家鱼类养殖场中鱼肠道内容物样品进行测定,结果表明共检出1种磺胺类、1种喹诺酮类、2种四环素类和3种大环内酯类抗生素,其中阿奇霉素(azithromycin,AZI)检出率较高。结论 该方法适用于鱼肠道内容物中32种抗生素残留的测定,并可进一步为高效液相色谱-串联质谱法在各类样品检测及分析等方面的研究提供科学指导及理论依据。

Objective To establish a method for the determination of 32 kinds of antibiotic residues in fish intestinal content by high performance liquid chromatography-tandem mass spectrometry. Methods It was determined that the chromatographic column was ACQUITY UPLC BEH C_(18)(2.1 mm×100 mm, 1.7 μm), acetonitrile and acidified acetonitrile were used as extraction solvents, purification by rapid column of veterinary drug residues,determination by high performance liquid chromatography-tandem mass spectrometry, matrix standard curve quantification. Results The limits of detection(LODs) of 32 kinds of antibiotics determined by this method were 0.2-0.5 μg/kg, and the limits of quantification(LOQs) were 1.0-1.5 μg/kg, the relative standard deviations(RSDs)were 1.2%-12.8%, the recoveries of 3 spiked concentrations were 79.5%-106.6%. On this basis, the method was used to determine the fish intestinal content samples of 5 fish farms, the results showed that 1 kind of sulfonamide,1 kind of quinolone, 2 kinds of tetracyclines and 3 kinds of macrolide antibiotics were detected, and the detection rate of azithromycin(AZI) was higher. Conclusion Based on the above conclusions, this method is suitable for the determination of 32 kinds of antibiotic residues in fish intestinal content, and can further provide scientific guidance and theoretical basis for the study of high performance liquid chromatography-tandem mass spectrometry in the detection and analysis of various samples.