固相萃取/超高效液相色谱-电喷雾串联质谱法检测酶制剂中3-硝基丙酸  

Determination of 3-Nitropropionic Acid in Zymin by Solid Phase Extraction Coupled with Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry

作　　者：张璐 乐爱山 郑玲 孔祥虹 

机构地区：[1]陕西出入境检验检疫局,陕西西安710068 [2]广西出入境检验检疫局,广西南宁530022

出　　处：《分析测试学报》2013年第6期747-752,共6页Journal of Instrumental Analysis

基　　金：国家质检总局科研项目(2011IK198)

摘　　要：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(1.8μm,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12.5～125μg/L范围内呈良好线性关系,相关系数大于0.993,定量下限为5.0μg/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。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.

关 键 词：固相萃取 超高效液相色谱-串联质谱 3-硝基丙酸 酶制剂 

分 类 号：O657.63[理学—分析化学] O611.63[理学—化学]