QuEChERS/液相色谱串联质谱法测定水产品中氯硝柳胺

Simultaneous determination of niclosamide in aquatic products by QuEChERS / liquid chromatography-tandem mass spectrometry

本文建立了QuEChERs／液相色谱一质谱／质谱（HPLC—MS／MS）测定水产品中氯硝柳胺残留量的分析方法。样品经氨化乙腈提取，C18吸附剂与中性氧化铝净化后，采用HPLC—MS／MS选择反应监测（SRM）负离子模式测定进行定性、定量分析。结果表明：在0．5～100ng／mL范围内，峰面积与浓度线性良好，相关系数为0．9996；氯硝柳胺检出限（LOD）为0．2μg/kg，定量限（LOQ）为0．4μg/kg，检测结果的相对标准偏差为4．33％～9．91％（n=5），平均加标回收率达到74．6％～92．1％。该方法具有较高的适用性和选择性，在水产品中氯硝柳胺的残留测定中具有很好的应用前景。

To establish an analytical method for the determination of niclosamide in aquatic products by QuEChERS/liquid chromatography-tandem mass spectrometry, the sample was extracted with acetonitril, the extract was cleaned up with C18 and Alumina-N, the mass spectrometer was operated in the negative ion mode using selected reaction monitoring for the qualitative and quantitative analysis.The linear ranges were from 0.5 to 100 ng/mL with a good linear relationship（ R2 =0.9996）.The detection limits of this method for niclosamide residues were 0.2μg/kg, and the limits of quantification were 0.4μg/kg.The relative standard deviations ranging from 4.33 % -9.91% （n = 5）and the average recovery rates were from74.6%-92.1%. The method proposed by this paper possessed higher applicability and selectivity. It is promising in real applications of determining the niclosamide residues in aquatic products.