色谱2013，Vol.31Issue(1)：22-26,5.DOI:10.3724/SP.J.1123.2012.07039
高效液相色谱-串联质谱法测定芽苗类蔬菜及其来源豆类中4种非法添加物的残留量
Determination of four kinds of illegal additive residues in sprouts and source beans by high performance liquid chromatography-tandem mass spectrometry
摘要
Abstract
A reversed-phase high performance liquid chromatography coupled with tandem mass spectrometric (LC-MS/MS) method was developed for the determination of 4-chlorophe-noxyacetic acid, 6-benzylaminopurine, enrofloxacin and norfloxacin residues in sprouts and source beans. The sample was extracted by acetonitrile containing 0. 1% acetic acid and concentrated. The chromatographic analysis was carried out on a C18 column with methanol and 0. 1% formic acid solution as the mobile phases in gradient elution program. The MS analysis was set in electrospray ionization mode and separated to two segments of positive and negative modes. The precursor ions were m/z 189. 9, 226. 1, 359. 9 and 320. 1 , while the product ions for quantification were m/z 127. 0, 91. 2, 315. 9 and 276. 2 for 4-chlorophenoxyacetic acid, 6-benzylaminopurine, enrofloxacin and norfloxacin, respectively. The calibration curves showed good linearity in the range of 5 - 200 μg/L with correlation coefficients more than 0. 995. The limits of detection (LODs) were 1 μg/kg and the limits of quantification (LOQs) were 5 μg/kg for the four compounds spiked in mung bean sprouts and mung beans. The recoveries of the four compounds spiked at three levels of 5. 0, 10. 0 and 20. 0 μg/kg ranged from 70% to 91%, with the relative standard deviations ( RSDs) less than 14%. The method established is accurate, sensitive, simple, and has considerable advantages in the analysis of the four kinds of illegal additive residues in sprouts and beans simultaneously.关键词
液相色谱-串联质谱/非法添加物/芽苗类蔬菜/豆类/残留Key words
liquid chromatography-tandem mass spectrometry (LC-MS/MS) / illegal additives/sprouts/ beans/ residues分类
化学化工引用本文复制引用
柳菡,沈伟健,沈崇钰,张睿,吴斌,殷耀,许蔚,桂茜雯,余可垚,龚玉霞,赵增运,林宏..高效液相色谱-串联质谱法测定芽苗类蔬菜及其来源豆类中4种非法添加物的残留量[J].色谱,2013,31(1):22-26,5.基金项目
国家质量监督检验检疫总局科技计划项目(2011KJ39,2012KJ31) （2011KJ39,2012KJ31）
科技部科技支撑项目(2011BAK10B04). （2011BAK10B04）
