Ki John, Ji Hye Young, Yoo Sung-Eun, Kim Sun Ok, Lee Dong Ha, Lim Hong, Lee Hye Suk
Faculty of Pharmaceutical Sciences, University of British Columbia, Vancouver, Canada.
Arch Pharm Res. 2002 Oct;25(5):647-51. doi: 10.1007/BF02976938.
An LC/MS/MS method for the simultaneous determination of a neuroprotective agent for ischemia-reperfusion damage, KR-31378 and its N-acetyl metabolite KR-31612 in human plasma was developed. KR-31378, KR-31612 and the internal standard, KR-31543 were extracted from human plasma by liquid-liquid extraction. A reverse-phase HPLC separation was performed on Luna phenylhexyl column with the mixture of acetonitrile-5 mM ammonium formate (55:45, v/v) as mobile phase. The detection of analytes was performed using an electrospray ionization tandem mass spectrometry in the multiple reaction monitoring mode. The lower limits of quantification for KR-31378 and KR-31612 were 2.0 ng/ml. The method showed a satisfactory sensitivity, precision, accuracy, recovery and selectivity.
建立了一种液相色谱/串联质谱法，用于同时测定人血浆中一种针对缺血再灌注损伤的神经保护剂KR-31378及其N-乙酰代谢物KR-31612。通过液液萃取从人血浆中提取KR-31378、KR-31612和内标KR-31543。在Luna苯基己基柱上进行反相高效液相色谱分离，以乙腈-5 mM甲酸铵（55:45，v/v）的混合物作为流动相。使用电喷雾电离串联质谱在多反应监测模式下对分析物进行检测。KR-31378和KR-31612的定量下限为2.0 ng/ml。该方法具有令人满意的灵敏度、精密度、准确度、回收率和选择性。
