摘要
基于固相萃取-超高效液相色谱串联质谱建立同时检测鸡粪中27种抗生素(12种磺胺类抗生素、8种喹诺酮类抗生素、5种四环素类抗生素和2种大环内酯类抗生素)的分析方法.样品中加入乙腈/磷酸-柠檬酸混合液及乙二胺四乙酸,经涡旋和超声提取,HLB固相萃取柱净化,采用高效液相色谱串联质谱测定.结果表明,27种抗生素在1—500μg·L^(‒1)范围内线性关系良好,相关系数r均大于0.994,检出限和定量限分别为0.1—0.8μg·kg^(‒1)和0.3—2.7μg·kg^(‒1).在50、100、500μg·kg^(‒1)的3个添加水平条件下,27种抗生素的平均回收率在66.1%—111.3%之间,相对标准偏差在2.3%—15.0%之间.采集4家养鸡场的鸡粪样品进行验证分析,发现鸡粪样中磺胺类、喹诺酮类和四环素类抗生素的检出浓度分别为未检出ND—28.1、ND—120.0、ND—4246.2μg·kg‒1.由此表明,该方法可用于鸡粪中多种抗生素的同时检测.
Simultaneous determination of 27 antibiotics(i.e.,12 sulfonamides,8 quinolones,5 tetracyclines and 2 macrolides)in chicken manure was investigated based on solid phase extraction(SPE)and ultra-high performance liquid chromatography tandem mass spectrometry(UPLCMS/MS).The samples were extracted by acetonitrile/phosphoric acid-citric acid mixture solution and ethylenediamine tetraacetic acid with the vortex and ultrasonic method,purified by HLB SPE cartridge,determined by UPLC-MS/MS.The results showed that linear relationship of 27 antibiotics in the range of 1—500μg·L^(‒1)was good with the correlation coefficient greater than 0.994.The limit of detection and quantitation of 27 antibiotics in the present method were 0.1—0.8μg·kg^(‒1)and 0.3—2.7μg·kg^(‒1),respectively.At three spiked levels(i.e.,50,100,500μg·kg^(‒1)),average recoveries of 27 antibiotics in chicken manure were in the range of 66.1%—111.3%with relative standard deviations of 2.3%—15.0%.Chicken manure samples from four chicken farms were collected for verification and analysis.It was found that the concentrations of sulfonamides,quinolones,and tetracyclines were in the range of ND(Not detected)—28.1,ND—120.0 and ND—4246.2μg·kg^(‒1),respectively.The results illustrate that the established method can be used for simultaneous detection of multiple antibiotics in chicken manure.
作者
李颖
黄鑫
邹子玉
贾春虹
赵尔成
邹洪涛
吴俊学
LI Ying;HUANG Xin;ZOU Ziyu;JIA Chunhong;ZHAO Ercheng;ZOU Hongtao;WU Junxue(Institute of Plant Protection,Beijing Academy of Agriculture and Forestry Science,Beijing,100097,China;College of Land and Environment,Shenyang Agricultural University,Shenyang,110866,China)
出处
《环境化学》
CAS
CSCD
北大核心
2023年第12期4185-4194,共10页
Environmental Chemistry
基金
北京市农林科学院创新能力建设项目(KJCX20210434)资助.
