阿维菌素粉中非法添加非泼罗尼检查方法的建立

Establishment of Detection Methods For Fipronil in Avermectin Powder

关键词:  液相色谱－串联质谱  阿维菌素粉  非泼罗尼

摘要:

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,使用C₁₈(100 mm×2.1 mm ,1.7 μm)色谱柱,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/mL范围内与峰面积呈良好的线性关系(r₂＝0.9995)；平均回收率为100.2%(n＝15),RSD为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。

Abstract:

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 0.025～20 ng/mL(r₂＝0.9995). The average recovery was 100.2% with RSD of 7.7%(n=15).This method was simple, accurate , quick and sensitive. It was suitable for detection of fipronil illegally adulterated in avermectin powder.