摘要
在气相色谱-串联质谱（GC-MS/MS）多反应监测（MRM）模式下,建立了对尿液中八角枫碱、芦竹碱、毒扁豆碱、毛果芸香碱、哈尔碱、氧化苦参碱、黄华碱、钩吻素子、钩吻碱、延胡索乙素、吴茱萸碱、血根碱、白屈菜红碱、士的宁和马钱子碱15种有毒生物碱的定性定量分析。对样品前处理、色谱、质谱条件进行了优化。在优化条件下，毒扁豆碱、哈尔碱、钩吻素子和士的宁在20-800 μg/L范围内线性关系良好，其余生物碱在40-800 μg/L范围内线性关系良好，相关系数均不小于0.993 2。在高、中、低3种加标水平下，除八角枫碱的平均回收率为60.0%-68.3%外，其余14种生物碱的平均回收率为81.9%-114.4%，各生物碱的相对标准偏差（RSD）不大于17.6%。方法的检出限（LOD）为4-20 μg/L，定量下限（LOQ）为10-40 μg/L。该方法操作简便、快捷、灵敏，适用于中毒患者尿液中有毒生物碱成分的检测。
A new and rapid method was developed and validated for the simultaneous analysis of 15 alkaloids,including anabasine,gramine,eserine,pilocarpine,harmine,oxymatrine,thermopsine,koumine,gelsemine,tetrahydropalmine,evodiamine,sanguinarine,chelerythrine,strychnine and brucine in urine.The conditions of extraction,chromatography and mass spectrometry were optimized,and the matrix effects of the alkaloids were also examined.The detection of target compounds was performed by gas chromatography-tandem mass spectrometry in multiple-reaction monitoring（MRM） mode.The content of each alkaloid was determined by the external standard method.The linear ranges were 20-800 μg/L for eserine,harmine,koumine and strychnine,and 40-800 μg/L for other target alkaloids with correlation coefficients not less than 0.993 2.The mean recoveries were in the range of 60.0%-68.3% for anabasine,and 81.9%-114.4% for other alkaloids.The relative standard deviations（RSDs） were not more than 17.6% at three spiked concentration levels.The limits of detection（LODs） and quantitation（LOQs） were 4-20 μg/L and 10-40 μg/L,respectively.The method was rapid,sensitive and easy operation,and was suitable for the determination of trace alkaloids in urine samples of poisonous persons.
出处
《分析测试学报》
CAS
CSCD
北大核心
2013年第9期1031-1037,共7页
Journal of Instrumental Analysis
基金
广东省科技计划资助项目(2008A030203010)
广州市越秀区科技计划资助项目(2009-PT-005)
关键词
气相色谱-串联质谱法
多反应监测
同时检测
尿液
有毒生物碱
gas chromatography - tandem mass spectrometry （ GC - MS/MS）
multiple-reaction mo- nitoring（MRM）
simultaneous determination
urine
toxic alkaloids
