色谱

色谱 ›› 2016, Vol. 34 ›› Issue (9): 860-867.DOI: 10.3724/SP.J.1123.2016.06010

• 研究论文 • 上一篇    下一篇

QuEChERS结合液相色谱-串联质谱法快速测定猪肉中多类兽药残留

张科明1, 梁飞燕2, 邓鸣1, 刘向红1, 许杨彪1, 赵庄1   

  1. 1. 广西食品药品检验所, 广西 南宁 530021;
    2. 广西-东盟食品药品安全检验检测中心, 广西 南宁 530021
  • 收稿日期:2016-06-05 出版日期:2016-09-08 发布日期:2016-08-26
  • 通讯作者: 赵庄
  • 基金资助:

    广西科技基础条件平台建设项目（12-112-01D）；广西食品药品检验所科研项目（KY-2016-02）.

Multi-residue determination of veterinary drugs in porcine muscle by QuEChERS and liquid chromatography-tandem mass spectrometry

ZHANG Keming1, LIANG Feiyan2, DENG Ming1, LIU Xianghong1, XU Yangbiao1, ZHAO Zhuang1   

  1. 1. Guangxi Institute for Food and Drug Control, Nanning 530021, China;
    2. Guangxi-Asean Center for Food and Drug Safety Control, Nanning 530021, China
  • Received:2016-06-05 Online:2016-09-08 Published:2016-08-26
  • Supported by:

    Science and Technology Infrastructure Program of Guangxi (No. 12-112-01D); Science and Technology Program of Guangxi Institute for Food and Drug Control (No. KY-2016-02).

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摘要：

采用改进的QuEChERS方法提取和净化猪肉样品，建立了同时测定磺胺类、磺胺类增效剂、β-受体激动剂、四环素类、喹诺酮类、金刚烷胺和性激素共7类35种兽药残留的液相色谱-串联质谱（LC-MS/MS）检测方法。样品经 Na2EDTA（乙二胺四乙酸）-Mcllvaine缓冲液-2.5%（体积分数）乙酸乙腈溶液提取，提取液经盐析后取乙腈相，用氨基（NH2）吸附剂分散固相萃取净化后，在电喷雾离子源正离子多反应监测（MRM）模式下进行测定，基质外标法定量。35种兽药在1.0～50.0 μg/L范围内线性关系良好，相关系数均大于0.996。在3个不同添加水平下的平均回收率为71.8%～113.5%，相对标准偏差为0.6%～9.8%（n=6），检出限和定量限分别为0.01～1.01 μg/kg和0.04～3.37 μg/kg。该方法操作简单，净化效果好，灵敏度高，适用于猪肉中兽药多残留的同时快速定性、定量分析。

关键词: QuEChERS, 多类兽药残留, 液相色谱-串联质谱法, 猪肉

Abstract:

A liquid chromatography-tandem mass spectrometric method with modified QuEChERS procedure for sample preparation was developed for the simultaneous determination of 7 classes of 35 veterinary drugs including sulfonamides, sulfonamide potentiators, beta-agonists, tetracyclines, amnatadine and sex hormones in porcine muscle. The drugs were extracted with 0.1 mol/L Na2EDTA (ethylene diamine tetraacetic acid)-Mcllvaine buffer solution and acetonitrile containing 2.5% (v/v) acetic acid, and then the extracts were purified using dispersive-solid phase extraction with NH2 sorbent, and finally analyzed by liquid chromatography-tandem mass spectrometry in multiple reaction monitoring mode via positive electrospray ionization. The correlation coefficients of the standard calibration curves for the 35 veterinary drugs were all above 0.996. The blank samples were spiked at three levels, and the average recoveries ranged from 71.8% to 113.5% with the relative standard deviations from 0.6% to 9.8% (n=6). The limits of detection and the limits of quantification were 0.01-1.01 μg/kg and 0.04-3.37 μg/kg respectively. The method developed is easy to operate, sensitive, with good purification effect and suitable for the determination of residues in porcine muscle.

Key words: liquid chromatography-tandem mass spectrometry (LC-MS/MS), multi-class multi-residue veterinary drugs, porcine muscle, QuEChERS

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