HPLC-MS/MS法测定家兔血液中的NNN及其代谢物

摘要

In order to accurately determine A'-nitroso nornicotine (NNN) and its metabolites in rabbit blood, a high-performance liquid chromatography/tandem mass spectrometry method was established by optimizing chromatographic conditions and mass spectrometric conditions and using NNN-d4 as an internal standard. The samples were successively pretreated by protein precipitation, separated by a Waters-HILIC column, and analyzed by tandem mass detector under multi-reaction monitoring (MRM) mode. The results showed that the recoveries of NNN and its metabolites ranged from 80% to 111% with the relative standard deviations (RSDs) of 0.5% to 8.62% and the limits of detection of 0.039 to 0.217 ng/mL. This method is simple, sensitive, rapid, and suitable for the analysis of NNN and its metabolites in blood.%为了准确测定家兔血液中的N-亚硝基降烟碱(NNN)及其代谢物,通过对色谱、质谱条件的优化和选择,建立了以NNN -d4为内标,通过沉淀蛋白的前处理操作以及Waters亲水相互作用色谱(HILIC)柱分离和多离子反应监测模式( MRM)测定大耳朵白兔血浆中NNN及其代谢物的HPLC-MS/MS方法.结果表明,NNN及其代谢物的相对标准偏差(RSD)、回收率和检测限分别为0.50％ ～ 8.62％,80％～111％和0.039 ～ 0.217 ng/mL.该方法简单、快速灵敏,适合于血液中NNN及其代谢物的检测.