色谱 ›› 2011, Vol. 29 ›› Issue (03): 217-222.DOI: 10.3724/SP.J.1123.2011.00217

• 研究论文 • 上一篇    下一篇

高效液相色谱-串联质谱法测定猪肉中的阿维菌素类、地克珠利、妥曲珠利及其代谢物残留

宫小明*, 孙军, 董静, 于金玲, 王洪涛   

  1. 潍坊出入境检验检疫局, 山东 潍坊 261041
  • 收稿日期:2010-11-18 修回日期:2011-01-06 出版日期:2011-03-28 发布日期:2011-03-28
  • 通讯作者: 宫小明,硕士,工程师,研究方向为农兽药物残留、真菌毒素及添加剂分析. T
  • 基金资助:

    山东检验检疫局科研基金项目(项目编号: SK201028).

Determination of avermectin, diclazuril, toltrazuril and metabolite residues in pork by high performance liquid chromatography-tandem mass spectrometry

GONG Xiaoming*, SUN Jun, DONG Jing, YU Jinling, WANG Hongtao   

  1. Weifang Entry-Exit Inspection and Quarantine Bureau, Weifang 261041, China
  • Received:2010-11-18 Revised:2011-01-06 Online:2011-03-28 Published:2011-03-28

摘要: 建立了猪肉中阿维菌素、伊维菌素、多拉菌素、莫西菌素、乙酰氨基阿维菌素等5种阿维菌素类药物以及地克珠利、妥曲珠利、妥曲珠利砜、妥曲珠利亚砜等4种均三嗪类药物及其代谢物残留的高效液相色谱-串联质谱分析方法。样品采用乙腈提取,ODS粉分散固相萃取净化,经Venusil ASB C18色谱柱(150 mm×2.1 mm, 3.0 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0.005~0.2 mg/L范围内线性关系良好,相关系数均大于0.990。猪肉基质中9种分析物在0.005、0.01、0.02 mg/kg加标水平下,回收率为73.2%~91.5%,相对标准偏差为12%~17%。该方法稳定、可靠,可满足猪肉中阿维菌素类、均三嗪类药物残留的检测与确证。

关键词: 阿维菌素类药物, 地克珠利, 高效液相色谱-串联质谱, 妥曲珠利及其代谢物, 猪肉

Abstract: A method for the determination of avermectin, ivermectin, doramectin, moxidectin, eprinomectin, diclazuril, toltrazuril and its two metabolite residues in pork was developed using QuEChERS method with high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS). The sample was extracted with acetonitrile and purified through QuEChERS method using ODS as the sorbent. The target compounds were separated on a Venusil ASB C18 column (150 mm×2.1 mm, 3.0 μm) and detected by HPLC-MS/MS. The linear ranges were 0.005~0.2 mg/L and the correlation coefficients were all above 0.990. The average recoveries and the relative standard deviations ranged from 73.2% to 91.5% and from 12% to 17% at the spiked levels of 0.005, 0.01 and 0.02 mg/kg for the 9 analytes in pork matrix. This method is reliable, and suitable for the determination of the residues of avermectin and related compounds in pork.

Key words: avermectin, diclazuril, pork, toltrazuril and its metabolites, high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS)