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
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摘要: 本文建立了Qu ECh ERS/液相色谱-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0.5100 ng/m L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。Abstract: 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 C_18 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 to100 ng / m L with a good linear relationship( R~2= 0.9996).The detection limits of this method for niclosamide residues were 0.2 μg / kg,and the limits of quantification were 0.4 μg / 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.