摘要
建立了液相色谱-串联质谱法测定人血浆中的苯达莫司汀（1）和活性代谢产物γ-羟基苯达莫司汀（2）,并考察2的同分异构体对测定的影响。使用Synergi Hydro-RP柱,以甲醇∶5mmol/L乙酸铵溶液（含0.1%甲酸）（54∶46）为流动相,流速梯度洗脱。采用电喷雾电离源,多反应监测模式,正离子检测。在人血浆中共检测到4种羟基代谢物（m/z374.1）,其中,2的3种同分异构体的峰面积之和不足其1%。人血浆中1和2在3~8 000 ng/ml和1.5~1 000 ng/ml范围内线性关系良好。1、2的日内和日间RSD小于6.0%和8.0%,准确度为96.2%~106.0%和98.6%~103.0%。
An LC-MS/MS method was established for the determination of bendamustine （1） and its active metabolite y-hydroxy bendamustine （2） in human plasma, and the effect of the isomers of 2 on the determination was also investigated. A Synergi Hydro-RP column was used, with the mobile phase of methanol ： 5 mmol/L ammonium acetate solution （containing 0.1% formic acid） （54 ： 46） by gradient flow programming. A multiple reaction monitoring （MRM） mode was applied in the positive mode for mass spectrometric detection. In metabolic profiles of 1 in human plasma, four hydroxylated metabolites （m/z 374.1） were observed, in which the total peak area of the three isomers was no more than 1% of that of 2. It was linear for 1 and 2 in the ranges of 3 - 8 000 ng/ml and 1.5 - 1 000 ng/ml, respectively. Their intra- and inter-day RSDs were within 6.0 % and 8.0 %, and their accuracies were 96.2 % - 106.0 % and 98.6 % - 103.0 %, respectively.
出处
《中国医药工业杂志》
CAS
CSCD
北大核心
2015年第8期866-870,共5页
Chinese Journal of Pharmaceuticals
