色谱

色谱 ›› 2019, Vol. 37 ›› Issue (5): 518-524.DOI: 10.3724/SP.J.1123.2018.11006

• 研究论文 • 上一篇    下一篇

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

余佩瑶1,2, 陈传胜1, 刘寒冰2, 邓艳玲2, 薛南冬2   

  1. 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
  • 收稿日期:2018-11-08 出版日期:2019-05-08 发布日期:2015-03-23
  • 通讯作者: 陈传胜,Tel:(0730)5644464,E-mail:65394814@qq.com;薛南冬,Tel:(010)84912638,E-mail:xuend@craes.org.cn
  • 基金资助:

    国家重点研发计划（2017YFD0800700，2016YFD0800202）.

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

YU Peiyao1,2, CHEN Chuansheng1, LIU Hanbing2, DENG Yanling2, XUE Nandong2   

  1. 1. College of Environmental Science and Engineering, Central South University of Forestry and Technology, Changsha 410000, China;
    2. Institute of Soil and Solid Waste, Chinese Research Academy of Environmental Sciences, Beijing 100012, China
  • Received:2018-11-08 Online:2019-05-08 Published:2015-03-23
  • Supported by:

    National key Research and Development Plan (Nos. 2017YFD0800700, 2016YFD0800202).

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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r2在0.9999~1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1.3~6.7 μg/kg，定量限为3.5~9.2 μg/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。

关键词: 高效液相色谱, 固相萃取, 抗生素, 畜禽粪便

Abstract:

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) H3PO4 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 (r2) of the standard curves were between 0.9999 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 μg/kg; and the limits of quantity were 3.5-9.2 μg/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.

Key words: antibiotic, chicken manure, high performance liquid chromatography (HPLC), solid phase extraction (SPE)

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