HPLC法快速测定饲料中硝基咪唑类药物的研究

Rapid Determination of Nitroimidazole Drugs in Feeds by HPLC Method

[目的]为建立一种检测饲料中硝基咪唑类药物的HPLC方法。[方法]提取饲料样品中的甲硝唑、二甲硝唑、罗硝唑和替硝唑,用Oasis MCX小柱进行净化后,以甲醇-水溶液为流动相,梯度洗脱,紫外检测波长为320 nm,进行HPLC测定。[结果]甲硝唑、罗硝唑、二甲硝唑和替硝唑的检测限分别为15.7、25.3、27.3和54.9μg/kg。在0.1～10.0μg/ml浓度范围内,4种硝基咪唑类药物色谱峰面积与浓度呈线性相关,相关系数为0.993～0.999,符合对饲料中抗生素分析的要求。4种硝基咪唑类药物平均回收率为82.5%～99.7%,符合对饲料中药物添加剂分析的准确度要求,变异系数为3.5%～14.0%,符合残留分析对精密度要求。[结论]该方法操作简单、结果准确,可用于测定饲料中硝基咪唑类药物的含量。

[Objective] The research aimed to establish a kind of HPLC method for detecting nitroimidazole drugs in feeds. [Method] Metronidazole, dimetfidazole, ronidazole and tinidazole were extracted from feed samples. They were purified by using Oasis MCX columella and determined with HPLC at the ultraviolet detection wavelength of 320 nm by taking methanol-water solution as mobile phase and using the technology of gradient elution. [Result] The detection limit for metronidazole, ronidazole, dimetridazole and tinidazole were 15.7, 25.3, 27.3 and 54.9 μg/kg respectively. In the concentration range of 0.1～10.0μg/ml, the chromatographic peak area of 4 kinds of nitroimidazole drugs showed linear correlation to their concentrations, with correlation coefficients of 0,993～0.999, which was accordant with the demands of antibiotics analysis in feeds, The average recovery of 4 kinds of nitroimidazole drugs were 82.5 %～99.7 % ,which was accordant with the accuracy requirement of analyzing drug additives in feeds. Their variation coefficients were 3.5 %～14.0 %, which was accordant with the precision requirement in residue analysis. [Conclusion] The method was simple to operate, with accurate results, which could be used for determining the contents of nitroimidazoles in feeds.