固相萃取-超高效液相色谱-串联质谱法测定猪肉中9种氨基糖苷类抗生素残留  

Determination of 9 Aminoglycosides Antibiotic in Pork by Solid Phase Extraction-Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry

作　　者：周寒琳 郭杭婷 张虹[1,2] 陈新旺 韩永和[1,2] 张勇[1,2] 贲玉婕 ZHOU Han-lin;GUO Hang-ting;ZHANG Hong;CHEN Xin-wang;HAN Yong-he;ZHANG Yong;BEN Yu-jie(College of Environmental and Resource Science,College of Carbon Neutral Modern Industry,Fujian Normal University,Fuzhou 350117,China;Fujian Key Laboratory of Pollution Control and Resource Reuse,Fujian Normal University,Fuzhou 350117,China;Department of Pulmonary and Critical Care Medicine,Fujian Medical University Union Hospital,Fuzhou 350001,China;Eastern Institute of Technology,Ningbo,Ningbo 315200,China)

机构地区：[1]福建师范大学环境与资源学院、碳中和现代产业学院,福建福州350117 [2]福建师范大学福建省污染控制与资源循环利用重点实验室,福建福州350117 [3]福建医科大学附属协和医院呼吸与危重症医学科,福建福州350001 [4]宁波东方理工大学(暂名),浙江宁波315200

出　　处：《化学试剂》2025年第1期86-91,共6页Chemical Reagents

基　　金：福建省自然科学基金面上项目(2022J01184)。

摘　　要：建立了猪肉样品中痕量氨基糖苷类抗生素(Aminoglycosides,AGs)(阿米卡星、安普霉素、潮霉素B、卡那霉素、巴龙霉素、核糖霉素、大观霉素、链霉素、妥布霉素)残留的检测方法。猪肉样品经过冷冻干燥、研磨后,加入150 mmol/L EDTA溶液和5%TCA溶液进行超声提取,经Oasis HLB柱净化后,采用BEH Z-HILIC色谱柱,进行超高效液相色谱-串联质谱分析。9种AGs在0.01~5μg/mL范围内线性关系良好,相关系数(R^(2))均大于0.999。猪肉样品中AGs的定量限为0.01~0.29μg/g。在低、中、高3种加标水平下,猪肉样品中AGs的平均加标回收率为79.91%~113.20%,相对标准偏差为1.26%~12.40%。该方法操作简单、灵敏度高,适用于猪肉中AGs残留的检测。The method was developed for the determination of trace aminoglycoside antibiotics(AGs)(Amikacin,Apramycin,Hygromycin B,Kanamycin,Paromomycin,Ribostamycin,Spectinomycin,Streptomycin,Tobramycin)residues in pork sample.The pork samples were freeze-dried and ground,then ultrasonically extracted by adding 150 mmol/L EDTA solution and 5%TCA solution,cleaned up by an Oasis HLB column,and then analyzed by ultra-performance liquid chromatography-tandem mass spectrometry.The linear relationships of the 9 AGs were in a good range of 0.01~5μg/mL(R^(2)≥0.999).The limits of quantitation were in the range of 0.01~0.29μg/g.At the three low,medium,and high spiking levels,the average spiking recovery rates of AGs in pork samples ranged from 79.91% to 113.20%,with relative standard deviations of 1.26%~12.40%.This method is simple,sensitive,and suitable for detecting of AGs residues in pork.

关 键 词：氨基糖苷类抗生素 固相萃取 超高效液相色谱-串联质谱法 猪肉 

分 类 号：O658[理学—分析化学]