食品研究与开发2025,Vol.46Issue(1) :160-170.DOI:10.12161/j.issn.1005-6521.2025.01.021

多次级相互作用检测猪肉中16种氨基糖苷类兽药残留

Residue Determination of 16 Aminoglycoside Veterinary Drugs in Pork by Multiple Secondary Interactions

梁飞燕 刘华文 吕敏 辛丽娜 黄玲 王丽
食品研究与开发2025,Vol.46Issue(1) :160-170.DOI:10.12161/j.issn.1005-6521.2025.01.021

多次级相互作用检测猪肉中16种氨基糖苷类兽药残留

Residue Determination of 16 Aminoglycoside Veterinary Drugs in Pork by Multiple Secondary Interactions

梁飞燕 1刘华文 1吕敏 1辛丽娜 1黄玲 1王丽1
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作者信息

  • 1. 广西-东盟食品检验检测中心,广西 南宁 530000
  • 折叠

摘要

该文建立一种基于以分配作用为主导,偶极相互作用、氢键作用、吸附作用、离子相互作用的多次级相互作用进行保留和分离的超高效液相色谱-质谱(ultra high performance liquid chromatography-mass spectrometry,UPLC-MS/MS)法,以测定猪肉中 16 种氨基糖苷类兽药残留量.样品采用磷酸盐缓冲液[pH4.0,含 2%三氯乙酸、0.04 mmoL/L乙二胺四乙酸二钠(ethylenediaminetetraacetic acid disodium salt,EDTA-2Na)、0.05 moL/L戊烷磺酸钠、0.05 moL/L己烷磺酸钠]提取,经HLB固相萃取柱(6 mL/200 mg)净化,通过Agilent Hilic plus(2.1 mm×100 mm,3.5µm)色谱柱的亲水相互作用进行保留和分离,三重四极杆串联质谱仪检测.在浓度 50~1 500 ng/mL线性良好,相关系数≥0.993,方法检出限为 3.8~19.7µg/kg,方法定量限为 12.5~65.8µg/kg,在 50、250、500µg/kg加标水平下,平均回收率为 79.6%~115.3%,相对标准偏差(relative standard deviation,RSD)为 0.8%~14.6%.该方法可以同时检测猪肉中 16 种氨基糖苷类抗生素,前处理简便,方法稳定性好、准确性、灵敏度高,可以满足猪肉中氨基糖苷类残留检测的监管需要.

Abstract

This study developed an ultra-high performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS)method based on multiple secondary interactions of partition,which was dominated,dipole interaction,hydrogen bonding,adsorption,and ion interaction for retention and separation to detect the resi-dues of 16 aminoglycoside veterinary drugs in pork.The samples were extracted by phosphate buffer solution(pH4.0)containing 2%trichloroacetic acid,0.04 mmoL/L ethylenediaminetetraacetic acid disodium salt(EDTA-2Na),0.05 moL/L sodium pentanesulfonate,and 0.05 moL/L sodium hexanesulfonate,purified by HLB solid-phase extraction column(6 mL/200 mg),retained and separated by an Agilent Hilic plus column(2.1 mm×100 mm,3.5µm)with the use of hydrophilic interaction,and detected by a triple quadrupole tan-dem mass spectrometer.There was a good linear correlation in the range of 50-1 500 ng/mL with correlation co-efficients≥0.993.The limit of detection was 3.8-19.7µg/kg,and the limit of quantitation was 12.5-65.8µg/kg.At the spiking levels of 50,250,500µg/kg,the average recovery was 79.6%-115.3%,and the relative stan-dard deviation(RSD)was 0.8%-14.6%.This method can simultaneously detect 16 aminoglycoside antibiotics in pork with simple pretreatment,good stability,high accuracy,and high sensitivity,which can meet the regulatory requirements for the detection of aminoglycoside residues in pork.

关键词

兽药残留/氨基糖苷类兽药/多次级相互作用/超高效液相色谱-质谱法/猪肉

Key words

veterinary drug residues/aminoglycoside veterinary drugs/multiple secondary interactions/ultra-high performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS)/pork

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出版年

2025
食品研究与开发
天津市食品研究所,天津市食品工业生产力促进中心

食品研究与开发

影响因子:0.561
ISSN:1005-6521
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