摘要
建立鸡球虫散、驱虫散中非法添加非泼罗尼的液相色谱检查方法。采用Agilent Eclipse Plus-C_(18)(3.5μm,4.6 mm×100 mm)色谱柱,以乙腈-水为流动相,梯度洗脱,二极管阵列检测器,波长采集190~400 nm,检查波长220 nm。通过色谱峰保留时间、峰纯度检查和光谱相似度检查对非泼罗尼进行定性,通过峰面积外标法进行定量。结果表明,方法检测限(LOD)为0.25 g/kg,在0.5 g/kg、2.0 g/kg、5.0 g/kg 3个添加浓度下,平均回收率为95.4%~101.5%,相对标准偏差为1.5%~2.5%,能够满足实际需求。本方法操作简单、检测快速、结果可靠,适用于以上2种制剂中非法添加非泼罗尼的定性定量检测。
The detection method of fipronil illegally addition in Jiqiuchongsan(medicine against chicken coccidiosis) and quchongsan(vermifuge) was established by HPLC-DAD. The isolation was performed on the Agilent Eclipse Plus-C_(18)(3.5μm,4.6×100 mm)chromatogramcolumn,gradient elution was carried out with water-acetonitrile as mobile phase. Used the diode array detector,The extraction wavelength was 220 nm. Fiproni was quantified by the retention time of chromatographic peak,peak purity testand spectra similarity,fiproni was quantitated by peak area. The results showed that the LOD was 0.25 g/kg,the average recovery rate ranged from 95.4 % ~ 101.5% at the level of 0.5,2.0,and 5.0 g/kg,the RSD was 1.5%~2.5%. This method was simple,fast and reliable,couldbe used as the determination method of quality and quantity.
引文
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