Chinese Journal of Chromatography

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Simultaneous determination of 19 quinolone residues in honey using high performance liquid chromatography-tandem mass spectrometry

DING Tao1*, SHEN Dongxu2, XU Jinzhong1, WU Bin1, CHEN Huilan1, SHEN Chongyu1, SHEN Weijian1, ZHAO Zengyun1, LIAN Hongzhen2   

  1. 1.Animal, Plant and Food Inspection Center (APFIC) of Jiangsu Entry-Exit Inspection and Quarantine Bureau, Nanjing 210001, China; 2.Key Laboratory of Analytical Chemistry for Life Science Education Ministry of China, Nanjing University, Nanjing 210008, China)
  • Received:2008-07-24 Revised:2008-09-30 Online:2009-01-30 Published:1983-03-25
  • Contact: DING Tao

Abstract: A method for the simultaneous analysis of 19 quinolone residues, enrofloxacin, ciprofloxacin, norfloxacin, ofloxacin, difloxacin, oxolinic acid, flumequine, sarafloxacin, sparfloxacin, danofloxacin, fleroxacin, marbofloxacin, enofloxacin, orbifloxacin, pipemidic acid, pefloxacin, lomefloxacin, cinofloxacin, and nalidixic acid in honey was developed by high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS). In comparison of the three different extraction methods, i.e. acid solution coupled with cation-exchange solid-phase extraction cartridge (PCX), neutral buffer solution coupled with a reversed-phase extraction cartridge (HLB) and alkali solution coupled with a strong anion-exchange solid-phase extraction cartridge (PAX), the third method was finally used. The cartridge was then applied to accumulate and purify the target analytes from the sample matrices in one step. The HPLC separation was performed on a C18 column with a linear gradient elution program of methanol and 0.1% formic acid solution as the mobile phase. Selective reaction monitoring (SRM) was used for the selective detection of 19 quinolones. The linearity of all the 19 quinolones in the range from 1 μg/L to 100 μg/L had correlation coefficient greater than 0.991. In the detection of spiked samples, the detection limit of the method was 1.0 μg/kg for all the 19 quinolones, and the recoveries were 71%-118% with the relative standard deviations of 4.2%-6.7%. Internal standard calibration was used for the quantitative analysis.

Key words: honey , quinolone drugs, high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS)