色谱

色谱 ›› 2013, Vol. 31 ›› Issue (10): 1028-1032.DOI: 10.3724/SP.J.1123.2013.03006

• 技术与应用 • 上一篇    

高效液相色谱法检测液态奶中的苯酚类和水杨酸苯胺类抗蠕虫药

王伟, 黄显会, 王辉, 严常燕, 孔祥凯   

  1. 华南农业大学国家兽药残留基准实验室, 广东 广州 510642
  • 收稿日期:2013-03-01 修回日期:2013-04-20 出版日期:2013-10-28 发布日期:2013-10-08
  • 通讯作者: 黄显会
  • 基金资助:

    2012年农业行业标准制修订项目(201214148).

Determination of phenolic and salicylanilide anthelmintics in liquid milk by high performance liquid chromatography

WANG Wei, HUANG Xianhui, WANG Hui, YAN Changyan, KONG Xiangkai   

  1. National Reference Laboratory of Veterinary Drug Residues, South China Agricultural University, Guangzhou 510642, China
  • Received:2013-03-01 Revised:2013-04-20 Online:2013-10-28 Published:2013-10-08

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摘要：

采用高效液相色谱法建立了硝碘酚腈、氯羟柳胺、氯氰碘柳胺、碘醚柳胺在液态奶中的多残留检测方法。取5 g样品,用含1%(v/v)三乙胺的乙腈提取,经MAX柱净化。以乙腈和0.02 mol/L乙酸铵水溶液(pH 4.0)作为流动相,经C18反相色谱柱分离后用紫外检测器检测,外标法定量。结果表明:空白加标奶样中4种药物在5~500 μg/kg范围内均呈现良好的线性关系,相关系数均大于0.99。空白加标奶样品的检出限(LOD)为3 μg/kg,定量限(LOQ)为5 μg/kg。硝碘酚腈、氯羟柳胺、氯氰碘柳胺、碘醚柳胺在1/2最高残留限量(MRL)、1倍MRL、2倍MRL添加水平下的平均回收率和相对标准偏差分别是92.20%~96.13%和5.55%~16.30%; 87.40%~94.74%和5.40%~12.21%; 86.97%~91.09%和2.67%~8.17%; 77.86%~95.36%和5.02%~13.15%。表明该检测方法简单,灵敏,适用于液态奶中水杨酸苯胺类多残留的定量分析检测。

关键词: 碘醚柳胺, 多残留, 高效液相色谱, 氯羟柳胺, 氯氰碘柳胺, 奶, 硝碘酚腈

Abstract:

An analytical method for the determination of nitroxynil, oxyclozanide, closantel and rafoxanide in liquid milk by high performance liquid chromatography (HPLC) has been established. The milk sample was extracted with acetonitrile containing 1% (v/v) triethylamine. The supernatant was purified by an anion exchange solid phase extraction column. The analyte was detected by ultraviolet detector after the HPLC separation on a C18 RP column. The mobile phase was composed of acetonitrile-0.02 mol/L ammonium acetate solution with pH 4.0. The linear ranges of the four drugs in the spiked blank milk samples were 5-500 μg/kg, and the correlation coefficients were higher than 0.99. The limits of detection (LOD) were 3 μg/kg, and the limits of quantification (LOQ) were 5 μg/kg. The average recoveries and relative standard deviations (RSDs) of nitroxynil, oxyclozanide, closantel and rafoxanide at the spiked levels of 1/2MRL (maximum residue limit), MRL and 2MRL ranged from 92.20% to 96.13%, 5.55% to 16.30%; 87.40% to 94.74%, 5.40% to 12.21%; 86.97% to 91.09%, 2.67% to 8.17%; and 77.86% to 95.36%, 5.02% to 13.15% respectively. The method is simple and sensitive for the quantification of phenolic and salicylanilide anthelmintics in liquid milk.

Key words: closantel, high performance liquid chromatography (HPLC), milk, multiresidue, nitroxynil, oxyclozanide, rafoxanide

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