液相色谱-串联质谱法测定阿维菌素粉中非法添加非泼罗尼的研究

Determination of Fipronil Illegally Adulterated in Avermectin Powder by Liquid Chromatography-tandem Mass Spectrometry

建立了阿维菌素粉中非法添加非泼罗尼的液相色谱-串联质谱检测方法,色谱柱为C18(100 mm×2.1 mm,1.7μm),以水-乙腈为流动相进行梯度洗脱,采用电喷雾离子源负离子检测模式(ESI-)和多反应监测(MRM)模式测定,外标法定量。结果表明,非泼罗尼进样浓度在0.025~20 ng/m L范围内与峰面积呈良好的线性关系(r2=0.9995);检出限和定量限分别为0.04 mg/g和0.1 mg/g;在0.1、1、30 mg/g三个添加水平下,回收率在84.6%~112.6%之间,相对标准偏差为1.0%~7.7%。本方法简便、准确、快速、灵敏,适用于阿维菌素粉中非法添加非泼罗尼的检测。

A detection method of fipronil illegally adulterated in avermectin powder was established by liquid chromatography-tandem mass spectrometric. The isolation was performed on a C18 column（ 100 mm × 2. 1 mm,1.7 μm）,gradient elution was carried out with water-acetonitrile as mobile phase. Electrospray negative ion source（ ESI-）,multiple reaction monitoring mod（ MRM）,external standard method were applied to samples analysis.The results showed that there was a good linear correlation between the peak areas and the concentrations of fipronil at the range of from 0.025 to 20 ng/m L（ r2= 0.9995）. The limit of detection and limit of quantification was 0.04 mg/g and 0.1 mg/g. The method validation was carried out at 0.1,1,30 mg/g,the recoverys were from84.6% to 112.6%,and the RSDs were from 1.0% to 7.7%.This method was simple,accurate,quick and sensitive.It was suitable for detection of fipronil illegally adulterated in avermectin powder.