摘要
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.
作者
丁奇
王建凤
冯月超
吴赞
马立利
刘佳
王颖
贾丽
高丽娟
邵鹏
王秋水
DING Qi;WANG Jian-Feng;FENG Yue-Chao;WU Zan;MA Li-Li;LIU Jia;WANG Ying;JIA Li;GAO Li-Juan;SHAO Peng;WANG Qiu-Shu(Institute of Analysis and Testing,Beijing Academy of Science and Technology,Beijing Center for Physical and Chemical Analysis,Beijing 100089,China)
出处
《食品安全质量检测学报》
CAS
北大核心
2022年第4期1141-1149,共9页
Journal of Food Safety and Quality
基金
北京市科学技术研究院分析测试研究所改革与发展项目(2021ZL0112)
北京市科学技术研究院市级财政项目(PXM2021_178305_000005)、北京市科学技术研究院市级财政项目(11000022T000000442954)、北京市科学技术研究院“北科萌芽”计划(11000022T000000455559)。
关键词
高效液相色谱-串联质谱法
肠道内容物
抗生素
固相萃取柱
high performance liquid chromatography-tandem mass spectrometry
intestinal content
antibiotics
solid phase extraction column
