Determination of 3-Nitropropionic Acid in Zymin by Solid Phase Extraction Coupled with Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry
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KeyWord:solid phase extraction  ultra performance liquid chromatography-tandem mass spectrometry  3-nitropropionic acid(3-NPA)  zymin
张璐,乐爱山,郑玲,孔祥虹 1.陕西出入境检验检疫局;2.广西出入境检验检疫局
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      A method was developed for the quantitation of 3-nitropropionic acid in zymin by high performance liquid chromatography-tandem mass spectrometry(LC-MS/MS).The analyte in samples was extracted with acetonitrile and the extract was purified with PSA solid phase extraction column.The separation of 3-nitropropionic acid was carried out on a Waters HSS T3 column by gradient elution using acetonitrile-water as mobile phase.The mass analyzer was performed in negative MRM mode.The result showed that the calibration curve of 3-nitropropionic acid was linear in the range of 12.5-125 μg/L with correlation coefficients more than 0993.The limit of quantitation(LOQ) was 5.0 μg/kg.The recoveries of 3-nitropropionic acid at different spiked levels ranged from 69.1% to 114.4% with relative standard deviations(RSDs) of 0.9%-8.9%.The real sample test showed that the method was simple,rapid and reliable.