建立了亲水相互作用色谱一串联质谱(HILIC—MS/MS)分析家兔血液中NNK及其代谢物的方法。以NNK—d。、NNAL—d,和HPB—d。为内标,血浆样品用乙腈沉淀蛋白后,直接进行HILIC分离和多反应监测(MRM)分析。结果表明,NNK及其代谢物的检出限在0.016~0.082ng/mL之间,r为0.9991~1.0000,加标回收率为76.9%~116.3%,日内精密度为0.53%~6.52%。该方法适合于同时分析血液中的NNK及其7种代谢物。
A method of determining NNK and its seven metabolites in rabbit blood with HILIC-MS/MS (hydrophilic interaction liquid chromatography tandem mass spectrometry) was established. Using NNK-d4, NNAL-d3 and HPB-d4 as internal standards, immediately after protein precipitating with acetonitrile, the plasma samples were separated by a HILIC column, then determined by mass spectrometry under multi-reaction monitoring (MRM) mode. The results showed that the limits of detection of NNK and its metabolites ranged from 0.016 to 0.082 ng/mL with r of 0.9991 to 1.0000, and the recoveries ranged from 76.9% to 116.3% with the intra-day precision of 0.53% to 6.52%. The method is suitable for the simultaneous analysis of NNK and its seven metabolites in blood.