色谱

色谱 ›› 2012, Vol. 30 ›› Issue (09): 883-888.DOI: 10.3724/SP.J.1123.2012.05023

• 研究论文 • 上一篇    下一篇

高效液相色谱-串联质谱法检测鸡肉中9种化学合成类抗球虫药多残留

施祖灏1, 张小燕1,2, 卜士金2, 陈大伟1, 蒲俊华1, 高玉时1*, 唐修君1   

  1. 1. 中国农业科学院家禽研究所 农业部家禽品质监督检验测试中心(扬州), 江苏 扬州 225125; 2. 扬州大学兽医学院, 江苏 扬州 225009
  • 收稿日期:2012-05-14 修回日期:2012-07-01 出版日期:2012-09-28 发布日期:2012-09-20
  • 基金资助:

    国家科技支撑计划项目（2012BAD39B04-3）、江苏省自然科学基金项目(BK2010299)和扬州市社会发展项目(2008040).

Simultaneous extraction and determination of nine chemically synthetic anticoccidial drug multi-residues in chicken meat using high performance liquid chromatography-tandem mass spectrometry

SHI Zuhao1, ZHANG Xiaoyan1,2, BU Shijin2, CHEN Dawei1, PU Junhua1, GAO Yushi1*, TANG Xiujun1   

  1. 1. Poultry Institute, Chinese Academy of Agricultural Sciences/Supervision, Inspection and Testing Center of Poultry Quality, Ministry of Agriculture (Yangzhou), Yangzhou 225125, China; 2. College of Veterinary Medicine, Yangzhou University, Yangzhou 225009, China
  • Received:2012-05-14 Revised:2012-07-01 Online:2012-09-28 Published:2012-09-20
  • Contact: 高玉时,研究员,研究方向为禽产品品质与安全. E-mail: gaoys100@sina.com.

PDF

526

被引次数

18

摘要： 建立了鸡肉中氯羟吡啶、二硝托胺、4,4′-二硝基均二苯脲(尼卡巴嗪代谢物)、磺胺氯吡嗪、磺胺喹口恶啉、地克珠利、妥曲珠利、妥曲珠利砜和妥曲珠利亚砜9种化学合成类抗球虫药多残留的高效液相色谱-串联质谱分析方法。样品采用2%乙酸酸化的乙腈/二甲亚砜(4:1, v/v)提取,150 mg二甲基十八碳硅烷粉(octadecylsilyl, ODS)、100 mg石墨化炭黑(graphitized carbon black, GCB)和100 mg弗罗里硅土(Florisil)吸附剂分散固相萃取净化,经Hypersil GOLD C18色谱柱(150 mm×4.6 mm, 5 μm)分离,电喷雾串联四极杆质谱多反应离子监测方式测定。9种分析物在20～150 μg/kg范围内线性关系良好,相关系数均大于0.995。样品基质中9种分析物在20、50和150 μg/kg加标水平下,平均回收率为81.5%～103.6%,相对标准偏差为4.5%～14.5%。该方法稳定、可靠,可满足鸡肉中化学合成类抗球虫药多残留的检测与确证。

关键词: 多残留, 高效液相色谱-串联质谱, 化学合成抗球虫药, 鸡肉

Abstract: A high performance liquid chromatography-tandem mass spectrometric (HPLC-MS/MS) method was developed for the simultaneous extraction and determination of multi-residues of nine chemically synthetic anticoccidial drugs in chicken meat. Toltrazuril-D3 was used as the internal standard. The sample was extracted by 15 mL acetonitrile/dimethyl sulfoxide (4:1, v/v, containing 2% acetic acid), cleaned-up by a QuEChERS (quick, easy, cheap, effective, rugged and safe) clean-up tube with 150 mg octadecylsilyl (ODS), 100 mg Florisil and 100 mg graphitized carbon black (GCB). After the concentration, the extract was analyzed by HPLC-MS/MS. The results showed that good linearity in the range of 20~150 μg/L for each target compound. The recoveries were between 81.5% and 103.6% with the relative standard deviations lower than 15%. The method is simple, rapid, and suitable to detect the chemically synthetic anticoccidial drug residues with high throughput.

Key words: chemically synthetic anticoccidial drugs, chicken meat, multi-residues, high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS)