摘要
建立了亲水作用色谱-串联质谱(HPLC-MS/MS)测定盐酸吗啉胍的方法,样品中的盐酸吗啉胍残留经三氯乙酸溶液沉淀和提取,加入庚烷磺酸钠离子对试剂后固相萃取柱净化,亲水作用色谱柱用于分离,正离子多反应监测模式检测(MRM),外标法定量。在添加含量5—100μg/kg范围内回收率为60%-107%;相对标准偏差(RSD)5.8%-12%;方法检出限(LOD)和定量下限(LOQ)分别为2、5μg/kg。方法可满足动物组织中盐酸吗啉胍定性、定量要求,该前处理和液相分离方法可用于其他强碱性化合物的测定。
A method has been developed to determine moroxydine hydrochloride in animal tissue by hydrophilic interaction chromatography with tandem mass spectrometry. Sample was precipitated and extracted by trichloroacetic acid solution. Sodium heptane sulfonate was used as the ion-pair reagent and the sample clean-up was achieved with solid-phase extraction column. Finally, it was determined by LC -MS/MS and multiple reactions monitoring, using positive electrospray ionization and external standard method. The recovery ranged from 60% to 107% fortified with 5 - 100 μg/kg moroxydine in various matrix and RSD was in the range of 5.8% - 12% ; the limits of detection(LOD) and limits of quantification(LOQ) were 2, 5 μg/kg. This method is suitable for determination of moroxydine in animal tissue.
出处
《分析测试学报》
CAS
CSCD
北大核心
2008年第4期437-439,共3页
Journal of Instrumental Analysis
基金
河南省科技攻关资助项目(0524430003)
关键词
盐酸吗啉胍
液相色谱-串联质谱
固相萃取
亲水作用色谱
moroxydine hydrochloride
HPLC - MS/MS
solid-phase extraction
hydrophilic interaction chromatography