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高效液相色谱-串联质谱法测定饲料中地克珠利的含量
侯轩
0
(浙江省兽药饲料监察所)
摘要:
建立了一种测定饲料中地克珠利的高效液相色谱-串联质谱方法。以乙腈提取样品中的待测物,正己烷除脂,离心后用高效液相色谱-串联质谱仪,选择多反应监测(MRM)、负离子模式进行定性和定量分析。结果表明,地克珠利在0.5~100 ng/mL浓度范围内线性关系良好,线性相关系数≥0.999,检出限为0.1 μg/kg,定量限为0.5 μg/kg。地克珠利在0.5、1和5 μg/kg三个添加水平下,三种饲料的平均加标回收率在79.2%~94.5%之间,相对偏差在1.7%~14.3%之间。本方法抗干扰能力强,操作简便,灵敏度高,适用于饲料中地克珠利的测定。
关键词:  饲料  地克珠利  高效液相色谱-串联质谱
DOI:
投稿时间:2016-01-08修订日期:2016-01-28
基金项目:
Determination of Diclazuril in feeds by High Performance Liquid Chromatography-Tandem Mass Spectrometry
(Zhejiang Provincial Supervisory Institute of Veterinary Drug)
Abstract:
An analytical HPLC-MS/MS method was established for determination of Diclazuril in feeds. The samples were extracted with acetonitrile, then defatted with n-hexane. The treated samples were analyzed by HPLC-MS/MS after centrifuged. The analysis was performed with Multi Reaction Monitor(MRM) in negative ion mode. The results indicated good lineartites in the concentration range from 0.5~100 ng/mL for Diclazuril, the correlation coefficient was over 0.999. The limit of detection(LOD) and the limit of quantitation(LOQ) were 0.1 and 0.5 μg/kg,respectively. While the spiked contents of Diclazuril standard at 0.5,1,5 μg/kg, the recoveries and relactive standard deviations(RSD) were in range of 79.2%~94.5% and 1.7%~14.3%,respectively. With the advantages of good anti-interference ability, rapidness and sensitivity, the method adapted to the determination of Diclazuril in feeds.
Key words:  feeds  Diclazuril  HPLC-MS/MS

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