分析测试学报2012，Vol.31Issue(6)：639-643,5.DOI:10.3969/j.issn.1004-4957.2012.06.002
亲水作用液相色谱-串联质谱测定水产品中的消毒剂残留
Determination of Aquaculture Disinfectants Residues in Aquatic Products by Hydrophilic Interaction Liquid Chromatography- Tandem Mass Spectrometry
摘要
Abstract
A new method for the determination of 3 aquaculture disinfectants in aquatic products u-sing hydrophilic interaction liquid chromatography -tandem mass spectrometry( LC - MS/MS) was established. The homogenized sample was extracted with acetonitrile 5% ammonia hydroxide (30: 70, by volume). Separation of analytes was performed using a SeQuant ZIC - HILIC hydrophilic in-teraction column by gradient elution after solid-phase extraction ( SPE) purification. The qualitative and quantitative analyses of 3 aquaculture disinfectants were operated by electrospray ionization mass spectrometry under the negative mode using multiple reaction monitoring ( MRM). Acetonitrile and water with 0. 1% formic acid and 10 mmol/L ammonium acetate were used as the mobile phase. The calibration curves were linear in the range of 0. 042 -2. 4 mg/L with correlation coefficients more than 0. 99. The average recoveries at three spiked concentration levels varied from 68% to 96% with relative standard deviations( RSDs) of 5. 9% - 10. 9% . The limit of detection( LOD, S/N≥3) and lim-it of quantitation ( LOQ, S/N≥10) were 0.015 mg/kg and 0.05 mg/kg, respectively. The real sample tests showed that the method was suitable for the determination of aquaculture disinfectants in aquatic products.关键词
亲水作用/液相色谱-串联质谱/水产肖毒剂/三氯生/二氯异氰尿酸/三氯异氰尿酸/水产品Key words
hydrophilic interaction/ liquid chromatography -tandem mass spectrometry (LC -MS/MS) / aquaculture disinfectants/ triclosan/ dichloroisocyanurate/ trichJoroisocyanurate/ aquatic products分类
化学化工引用本文复制引用
黄晓兰,罗辉泰,吴惠勤,朱志鑫,黄芳,林晓珊..亲水作用液相色谱-串联质谱测定水产品中的消毒剂残留[J].分析测试学报,2012,31(6):639-643,5.基金项目
广东省科技计划重点专项"农产品检测监控与追溯技术研究与示范"资助项目(2009A020101004) （2009A020101004）
