分散固相萃取净化-高效液相色谱-串联质谱法测定鱼体中地克珠利残留量

doi:10.7506/spkx1002-6630-201614031

摘要/Abstract

摘要：

建立分散固相萃取净化-高效液相色谱-串联质谱法测定鱼体中地克珠利残留量的分析方法。样品经无水硫酸钠脱水，乙腈超声提取并减压浓缩，正己烷去脂，基质分散固相萃取净化，以电喷雾离子源负离子扫描模式进行质谱分析，内标法定量。结果表明，地克珠利在1～100 μg/L范围内线性关系良好，相关系数R2大于0.999。地克珠利添加水平为1.00～50.0 μg/kg时，平均回收率在95.4%～108%之间，批内和批间变异系数均小于15%。地克珠利的检出限为0.50 μg/kg。本方法灵敏、高效、简单、重复性好，能满足鱼体中地克珠利残留量的检测要求。

关键词: 分散固相萃取, 高效液相色谱-串联质谱, 鱼, 地克珠利

Abstract:

A method has been developed for the determination of diclazuril in fish by high performance liquid
chromatography-tandem mass spectrometry (HPLC-MS/MS) with dispersive solid phase extraction. Samples were
dehydrated with anhydrous sodium sulfate, and extracted with acetonitrile. Then the extracts were concentrated under
vacuum condition. The samples were degreased with hexane and cleaned up by dispersive solid phase extraction, analyzed
by HPLC-MS/MS and quantified with internal standard method. Electrospray ionization was applied and operated in the
negative ion mode. The calibration curve showed good linearity between peak area and the concentration of diclazuril
in the range of 1–100 μg/L with a correlation coefficient over 0.999. The average recoveries from spiked sample at the
three concentrations of 1.00, 5.00 and 50.0 μg/kg ranged from 95.4% to 108% with intra- and inter-batch relative standard
deviations below 15%. The limit of detection (LOD) for diclazuril was 0.50 μg/kg. This efficient and simple method could
be used to identify and quantify diclazuril in fish with satisfactory sensitivity and repeatability.

Key words: dispersive solid phase extraction, high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS), fish, diclazuril

中图分类号:

O657.63

邢丽红，孙伟红，孙晓杰，李兆新，郭江涛. 分散固相萃取净化-高效液相色谱-串联质谱法测定鱼体中地克珠利残留量[J]. 食品科学, doi: 10.7506/spkx1002-6630-201614031.

XING Lihong, SUN Weihong, SUN Xiaojie, LI Zhaoxin, GUO Jiangtao. Determination of Diclazuril in Fish by High Performance Liquid Chromatography-Tandem Mass Spectrometry with Dispersive Solid Phase Extraction[J]. FOOD SCIENCE, doi: 10.7506/spkx1002-6630-201614031.

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