固相萃取-高效液相色谱法同时测定鸡粪中四环素类、喹诺酮类和磺胺类抗生素  

Simultaneous determination of tetracyclines, fluoroquinolones, and sulfonamides in chicken manure using solid-phase extraction and high performance liquid chromatography

作　　者：余佩瑶 陈传胜 刘寒冰[2] 邓艳玲 薛南冬[2] YU Peiyao;CHEN Chuansheng;LIU Hanbing;DENG Yanling;XUE Nandong(College of Environmental Science and Engineering,Central South University of Forestry and Technology,Changsha 410000,China;Institute of Soil and Solid Waste,Chinese Research Academy ofEnvironmental Sciences,Beijing 100012,China)

机构地区：[1]中南林业科技大学环境科学与工程学院,湖南长沙410004 [2]中国环境科学研究院土壤与固体废物环境研究所,北京100012

出　　处：《色谱》2019年第5期518-524,共7页Chinese Journal of Chromatography

基　　金：国家重点研发计划(2017YFD0800700;2016YFD0800202)~~

摘　　要：建立了一种高效、低成本的固相萃取-高效液相色谱(SPE-HPLC)同时测定鸡粪中6种常见抗生素(2种四环素类、2种喹诺酮类和2种磺胺类)的分析方法。样品经EDTA-McIlvaine缓冲液和有机混合提取液(甲醇-乙腈-丙酮,2∶2∶1, v/v/v)提取,过HLB固相萃取柱净化,甲醇-二氯甲烷(7∶3, v/v)洗脱,高效液相色谱-二极管阵列检测器测定,检测波长λ=270 nm,柱温32℃,流动相为乙腈-0.7%(v/v)磷酸水溶液。该方法在0.5～100 mg/L质量浓度范围内的标准曲线相关系数r^2在0.999 9～1之间,样品加标回收率在70.0%～116.3%之间,相对标准偏差为1.2%～16.6%。方法检出限为1.3～6.7μg/kg,定量限为3.5～9.2μg/kg。应用该方法对辽宁省抚顺市某养鸡场当天的鸡粪进行检测,诺氟沙星和恩诺沙星(喹诺酮类)含量为未检出～9.23 mg/kg和1.57～7.69 mg/kg,磺胺二甲嘧啶(磺胺类)含量为2.02～13.05 mg/kg,磺胺甲恶唑、土霉素和四环素未测出。A highly efficient and economic method for the simultaneous determination of six common antibiotics (two tetracyclines,two quinolones,and two sulfonamides) in chicken manure was developed by using solid-phase extraction and high performance liquid chromatography (SPE-HPLC).The samples were extracted by using a mixture of the EDTA-McIlvaine buffer and a mixed organic extractant (methanol-acetonitrile-acetone,2 ∶ 2 ∶ 1,v/v/v),cleaned by a hydrophile-lipophile balance (HLB) cartridge,eluted by methanol-dichloromethane (7 ∶ 3,v/v),and separated by HPLC with an acetonitrile-0.7%(v/v) H 3PO 4 aqueous solution as the mobile phase.The detection wavelength and temperature of the chromatographic column were 270 nm and 32 ℃,respectively.All antibiotics showed great linear relationships in the range of 0.5-100 mg/L;the correlation coefficients ( r 2) of the standard curves were between 0.999 9 and 1;the recoveries of antibiotics were between 70.0% and 116.3%;and the relative standard deviations were between 1.2% and 16.6%.The limits of detection were 1.3-6.7 μ g/kg;and the limits of quantity were 3.5-9.2 μ g/kg.This method was used to detect antibiotics in chicken manure from a hennery in Fushun,Liaoning Province.The contents of norfloxacin and enrofloxacin (quinolones) were from not detected to 9.23 mg/kg and 1.57-7.69 mg/kg,respectively,that of sulfamethazine (sulfonamides) were 2.02-13.05 mg/kg,while sulfamethoxazole,oxytetracycline,and tetracycline were undetectable.

关 键 词：固相萃取 高效液相色谱 抗生素 畜禽粪便 

分 类 号：O658[理学—分析化学]