Determination of four kinds of illegal additive residues in sprouts and source beans by high performance liquid chromatography-tandem mass spectrometry
Author(s) -
Liu Han,
Bin Wu,
Yin Yao,
Wei Xu,
Qianwen Gui,
Keyao YU,
Yuxia Gong,
Zengyun Zhao,
HongPing Lin,
Weijian Shen,
Chongyu Shen,
Rui Zhang
Publication year - 2013
Publication title -
chinese journal of chromatography
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.171
H-Index - 19
eISSN - 1872-2059
pISSN - 1000-8713
DOI - 10.3724/sp.j.1123.2012.07039
Subject(s) - chromatography , chemistry , formic acid , electrospray ionization , mass spectrometry , tandem mass spectrometry , acetic acid , selected reaction monitoring , high performance liquid chromatography , electrospray , liquid chromatography–mass spectrometry , detection limit , enrofloxacin , biochemistry , ciprofloxacin , antibiotics
A reversed-phase high performance liquid chromatography coupled with tandem mass spectrometric (LC-MS/MS) method was developed for the determination of 4-chlorophenoxyacetic 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 microg/L with correlation coefficients more than 0.995. The limits of detection (LODs) were 1 microg/kg and the limits of quantification (LOQs) were 5 microg/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 microg/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.
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