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 5.0μg/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.%采用高效液相色谱-电喷雾串联质谱对酶制剂中的3-硝基丙酸进行定性、定量分析.样品经乙腈提取,PSA固相萃取柱净化后,以Waters HSS T3柱(1.8 μm,2.1 mm× 100 mm)分离,乙腈和水为流动相,负离子模式扫描.结果表明,3-硝基丙酸在12.5～125 μg/L范围内呈良好线性关系,相关系数大于0.993,定量下限为5.0 μg/kg.在低、中、高3个加标水平下,3-硝基丙酸的回收率为69.1％～114.4％,相对标准偏差(RSD)为0.9％～8.9％.对酶制剂样品的测定表明该方法简便、快速,检测结果可靠.
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