摘要
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.
出处
《食品工业科技》
CAS
CSCD
北大核心
2016年第23期316-318,323,共4页
Science and Technology of Food Industry
关键词
氯硝柳胺
QUECHERS
液相色谱-质谱/质谱法
水产品
niclosamide
QuEChERS
liquid chromatography - mass spectrometry/mass spectrometry
aquatic products