色谱

色谱 ›› 2013, Vol. 31 ›› Issue (10): 1010-1015.DOI: 10.3724/SP.J.1123.2013.03048

• 技术与应用 • 上一篇    下一篇

固相萃取-高效液相色谱-串联质谱法测定畜禽粪便中的残留抗生素

王丽1,2, 钟冬莲1, 陈光才1, 汤富彬1, 宋秋华3, 张建锋1   

  1. 1. 中国林业科学研究院亚热带林业研究所, 浙江 富阳 311400;
    2. 江西理工大学冶金与化学工程学院, 江西 赣州 341000;
    3. 江西理工大学资源与环境工程学院, 江西 赣州 341000
  • 收稿日期:2013-03-27 修回日期:2013-05-14 出版日期:2013-10-28 发布日期:2013-10-08
  • 通讯作者: 陈光才
  • 基金资助:

    浙江省公益技术项目(2010C33188).

Determination of antibiotic residues in manure by liquid chromatography-tandem mass spectrometry coupled with solid phase extraction

WANG Li1,2, ZHONG Donglian1, CHEN Guangcai1, TANG Fubin1, SONG Qiuhua3, ZHANG Jianfeng1   

  1. 1. Research Institute of Subtropical Forestry, Chinese Academy of Forestry, Fuyang 311400, China;
    2. School of Metallurgy and Chemistry Engineering, Jiangxi University of Science and Technology, Ganzhou 341000, China;
    3. College of Resources and Environmental Engineering, Jiangxi University of Science and Technology, Ganzhou 341000, China
  • Received:2013-03-27 Revised:2013-05-14 Online:2013-10-28 Published:2013-10-08

PDF

276

被引次数

23

摘要：

建立了固相萃取-高效液相色谱-串联质谱法(HPLC-MS/MS)同时测定畜禽粪便中四环素类化合物(四环素、金霉素、土霉素)、喹诺酮类化合物(诺氟沙星、环丙沙星、洛美沙星)和磺胺二甲嘧啶7种抗生素的检测方法。样品中的抗生素用含有甲醇、乙酸和水(6:3:1, 体积比)的混合溶液提取后,经HLB固相萃取小柱纯化富集,采用Symmetry C18色谱柱分离,0.3%甲酸水溶液和0.3%甲酸乙腈溶液作为流动相进行梯度洗脱,电喷雾正离子(ESI+)模式电离,多反应监测(MRM)模式检测,外标法定量。结果表明,四环素类化合物和喹诺酮类化合物在50~1000 μg/L、磺胺二甲嘧啶在5~100 μg/L的范围内具有良好线性。3倍信噪比下,四环素类化合物、喹诺酮类化合物和磺胺二甲嘧啶的检出限分别为0.25~7.18、0.15~3.16和0.04 μg/kg。在猪粪和鸡粪样品中添加0.1~10 μg/g水平的四环素类化合物、喹诺酮类化合物和磺胺二甲嘧啶,其平均添加回收率为40%~124%,相对标准偏差(RSD)为3.0%~9.5%。采用该方法对部分养殖场的猪粪和鸡粪进行了检测,结果表明,四环素类化合物均有不同程度的检出,喹诺酮类化合物和磺胺二甲嘧啶有部分检出。该方法具有灵敏度和准确度高的特点,可满足畜禽粪便中四环素类化合物、喹诺酮类化合物及磺胺二甲嘧啶的检测。

关键词: 高效液相色谱-串联质谱, 固相萃取, 鸡粪, 抗生素, 猪粪

Abstract:

A method was developed for the simultaneous determination of tetracyclines (TCs), quinolones (QUs) and sulfadimidine (SM2) in pig manure and chicken dung by a combined high performance liquid chromatography (HPLC) and tandem mass spectrometry (MS/MS) detection coupled with solid phase extraction. The residual antibiotics in manure were extracted with the mixture of methanol, acetic acid and water with the volume ratio of 6:3:1, enriched and purified by a hydrophilic lipophilic balance (HLB) solid-phase extraction cartridge. The C18 chromatographic column was used to complete the separation of the analytes which were detected in multiple reaction monitoring (MRM) mode via positive electrospray ionization (ESI+). The external standard calibration curves were used for the quantification. All the antibiotics were determined with an excellent linear relationship from 50 to 1000 μg/L for TCs and QUs, and from 5 to 100 μg/L for SM2. The limits of detection for TCs, QUs and SM2 were 0.25-7.18, 0.15-3.16 and 0.04 μg/kg, respectively. The recoveries of TCs, QUs and SM2 in pig manure and chicken dung were 40%-124% at the spiked levels from 0.1 to 10 μg/g (RSDs ranged from 3.0% to 9.5%, n=6). The method was successfully applied to determine the antibiotics in pig manure and chicken dung samples. The method has high accuracy and sensitivity for the determination of TCs, QUs and SM2 in pig manure and chicken dung.

Key words: antibiotics, chicken dung, high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS), pig manure, solid phase extraction (SPE)

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