HILIC-MS/MS测定家兔血液中的NNK及其7种代谢物

Determination of NNK and its 7 Metabolites in Rabbit Blood with HILIC-MS/MS

摘要: 建立了亲水相互作用色谱-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-d₄、NNAL-d₃和HPB-d₄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0.016~0.082 ng/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。

Abstract: 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.