分析测试学报2017，Vol.36Issue(11)：1357-1362,6.DOI:10.3969/j.issn.1004-4957.2017.11.011
分散固相萃取净化/高效液相色谱-串联质谱法测定水产品中的5种硝基咪唑类药物残留
Determination of Five Nitromidazoles in Aquatic Products by High Performance Liquid Chromatography-Tandem Mass Spectrometry Combined with Dispersive Solid Phase Extraction
励炯 1孙岚 1王红青 1邱红钰 1康健2
作者信息
- 1. 杭州市食品药品检验研究院,浙江杭州310017
- 2. 岛津技迩(上海)商贸有限公司,上海200052
- 折叠
摘要
Abstract
A high performance liquid chromatography-tandem mass spectrometric(HPLC-MS/MS) method was developed for the determination of five nitromidazoles in aquatic products.Samples were extracted with acetonitrile containing 0.1％ (by volume) ammonium hydroxide,and then purified with a mixture of anhydrous sodium sulfate,C18-N and NH2-PSA.The analysis was performed by an HPLC-MS/MS system with Merck Chromolith Performance RP-18e(4.6 mm × 100 mm) column.The mobile phase consisted of methanol and 0.1％ (by volume) formic acid solution by gradient elution,and multiple reaction monitoring(MRM) mode with positive electrospray ionization was used.The effects of the dosages of ammonium hydroxide in extractant and anhydrous sodium sulfate,C1s-N and NH2-PSA in cleaning-up agent were studied.Under the optimized analytical conditions,the calibration curves for five nitromidazoles were linear in the concentration range of 20-500 μg/L with their correlation coefficients(r2) not less than 0.998 9.The recoveries at three concentrations ranged from 77.2％ to 94.8％ with the LOQs of 0.7-2.0 μg/kg.The method is suitable for the determination of 5 nitromidazoles in aquatic products.关键词
高效液相色谱/串联质谱/分散固相萃取/硝基咪唑/水产品Key words
high performance liquid chromatography/tandem mass spectrometry/dispersive solid phase extraction/nitromidazole/aquatic product分类
化学化工引用本文复制引用
励炯,孙岚,王红青,邱红钰,康健..分散固相萃取净化/高效液相色谱-串联质谱法测定水产品中的5种硝基咪唑类药物残留[J].分析测试学报,2017,36(11):1357-1362,6.
