摘要
本文应用QuEChERS前处理技术,结合高效液相色谱-高分辨质谱技术,对残留在生乳中磺胺类、大环内酯、林可酰胺、酰胺醇、青霉素5类32种兽药的同时测定进行了研究。本方法以1%氨水乙腈和1%乙酸乙腈为萃取溶剂,无水硫酸钠为脱水剂,C18和PSA为吸附剂,甲醇-0.1%甲酸水(1:9,V/V)为再溶解溶液。用Hypersil GOLD25002-102130 C18柱层析分离,流动相为0.1%甲酸水溶液和甲醇溶液梯度洗脱,Q-Exactive高分辨质谱,正负离子交换采集,外标法定量。该方法在质量浓度为0.5~100 ng/mL内线性良好,32种兽药残留的相关系数r大于0.995。加入5、20、50μg/kg(氯霉素、氟苯尼考1、5、20μg/kg)测定三种不同质量浓度加标样品,回收率为60.1%~116.7%,RSD为1.2%~9.7%。该方法的精密度和重复性良好。
QuEChERS pre-processing technology combined with high-performance liquid chromatography-high resolution mass spectrometry technology,the simultaneous determination of 32 veterinary drugs such as sulfonamides,macrolides,lincosamide,amide alcohol and penicillin in raw milk residues were studied. This method used 1% ammonia acetonitrile and 1% acetonitrile acetic acid as extraction solvents,anhydrous sodium sulfate as desiccant,C18 and PSA as adsorbents for purification and concentration,methanol-0.1% formic acid water(1:9,V/V) redissolve solution. Then it was separated by Hypersil GOLD25002-102130 C18 column chromatography,the mobile phase was 0.1% methanol aqueous solution and formic acid solution gradient elution,Q-Exactive high resolution mass spectrometry,positive and negative ion exchange acquisition mode electrospray,external standard method for quantification. The method had a good linearity in the mass concentration range of 0.5 ~ 100 ng/mL,and the correlation coefficient r of 32 kinds of veterinary drug residues was greater than 0.995. Adding 5,20,50 mg/kg(chloramphenicol,florfenicol1,5,20 μg/kg) to determine three different mass concentrations of spiked samples,the recovery rate was between 60.1% ~ 116.7%,RSD was 1.2% ~ 9.7%. The precision and repeatability of this method were good.
作者
高娃
徐艳伟
王志峰
吴云芳
GAO Wa;XU Yanwei;WANG Zhifeng;WU Yunfang(Xilingol Vocational College,Xilinhot,Inner Mongolia 026000,China;Xilingol League Center for Disease Control and Prevention,Xilinhot,Inner Mongolia 026000,China)
出处
《中国饲料》
北大核心
2022年第7期67-75,共9页
China Feed
基金
锡林郭勒职业学院科研课题(ZD-2020-07)。
关键词
生乳
QUECHERS
四极杆/静电场轨道阱高分辨质谱
兽药残留
raw milk
QuEChERS
quadrupole/electrostatic field orbitrap high-resolution mass spectrometry
veterinary drug residue
