HPLC-PDA法测定3种兽药中非法添加非泼罗尼

Determination of Fipronil in Veterinary Drug by HPLC-PDA

关键词:  阿维菌素粉  甲基吡啶磷可湿性粉  环丙氨嗪预混剂  非泼罗尼  峰纯度检查  光谱相似度检查  高效液相色谱法

Key words:  avermectin powder  azamethiphos wettable powder, cyromazine premix , fipronil, peak purity test  spectrum similar test  HPLC

摘要:

建立了3种兽药中非法添加非泼罗尼的HPLC-PDA检查方法。采用十八烷基硅烷键合硅胶为填充剂；以水-乙腈为流动相,梯度洗脱；二极管阵列检测器,提取波长为220 nm。通过液相色谱保留时间、峰纯度检查和光谱相似度检查对非法添加物进行确证。结果表明,该色谱条件下非泼罗尼与其他物质分离良好。非泼罗尼在阿维菌素粉、甲基吡啶磷可湿性粉、环丙氨嗪预混剂中的平均回收率分别为100.0%(RSD=1.6%)、108.7%(RSD=1.1%)、109.3%(RSD=1.2%)。本方法简便、准确、可靠,可用于检查以上3种兽药中非法添加的非泼罗尼。

Abstract:

A method for the determination of fipronil in three kinds of veterinary drug was developed by the high performance liquid chromatography with photo-diode array detector (HPLC-PDA). It was tested with C18 column, using gradient elution with water and acetonitrile as the mobile phase. The extract wavelength was 220 nm. Retention time, peak purity test and spectrum similar test were used to identify fipronil. Results showed that fipronil and other materials were finely separated. The mean recoveries of fipronil in avermectin powder, azamethiphos wettable powder and cyromazine premix were 100.0%(RSD=1.6%), 108.7%(RSD=1.1%), 109.3%(RSD=1.2%) respectively. In conclusion, the method is simple, accurate and reliable for the determination of fipronil in the three kinds of veterinary drug.