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Simultaneous determination of 19 quinolone residues in honey using high performance liquid chromatography-tandem mass spectrometry
DING Tao, SHEN Dongxu, XU Jinzhong, WU Bin, CHEN Huilan, SHEN Chongyu, SHEN Weijian, ZHAO Zengyun, LIAN Hongzhen
2009, 27 (1):
34-38.
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.
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