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阿维菌素粉中非法添加非泼罗尼检查方法的建立
杨修镇,陈玲,尹伶灵,刘少宁,牛华星,张呈军
0
(1.山东省兽药质量检验所;山东省畜产品质量安全监测与风险评估重点实验室)
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。
关键词:  液相色谱-串联质谱  阿维菌素粉  非泼罗尼
DOI:
投稿时间:2017-09-13修订日期:2018-03-05
基金项目:
Establishment of Detection Methods For Fipronil in Avermectin Powder
(Shandong Provincial Veterinary Medicine Supervision Institute)
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.
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