期刊
CHINESE JOURNAL OF CHROMATOGRAPHY
卷 31, 期 10, 页码 934-938出版社
SCIENCE PRESS
DOI: 10.3724/SP.J.1123.2013.01048
关键词
liquid chromatography-tandem mass spectrometry (LC-MS/MS) hydrophilic interaction chromatography (HILIC); dispersion solid phase extraction (DSPE); ribavirin; quick growth chicken; chicken products
An analytical method was developed for the determination of total residues of ribavirin and its phosphorylated metabolites in chicken and its products by hydrophilic interaction chromatography-tandem mass spectrometry. The samples were extracted with acetonitrile containing 1% (v/v) acetic acid under ultrasonic condition and then enzymatically hydrolysed with acid phosphatase at 37 degrees C. After liposoluble substances being removed with hexane, C-18 and PSA dispersion solid phase extraction (DSPE) was introduced to cleanup procedures. The separation was performed on an ultra-performance hydrophilic interaction chromatographic (HILIC) amide column under a gradient elution using acetonitrile and 0.1% formic acid. The analytes were detected in the positive electrospray ionization and multi-reaction monitoring (MRM) mode. In the range of 1-200 mu g/kg, the correlation coefficient was greater than 0.999. The limit of detection (LOD, S/N >= 3) was 1 mu g/kg and the limit of quantification (LOQ, S/N >= 10) was 5 mu g/kg. The recoveries of ribavirin spiked at three levels ranged from 67.8% to 112.7% with the relative standard deviations (RSDs) of 6.1%-13.6%. The results of the determination of ribavirin in various real samples showed that the method is simple, rapid, accurate and suitable for the determination of total residues of ribavirin and its metabolites in chicken and its products.
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