Xie Xu, Li Yongning, Gao Dongna, Zhang Yu, Ren Yanbo
Biomed Chromatogr. 2014 Sep;28(9):1229-34. doi: 10.1002/bmc.3151.
Euphol is a potential pharmacologically active ingredient isolated from Euphorbia kansui. A simple, rapid, and sensitive method to determine euphol in rat plasma was developed based on liquid chromatography-tandem mass spectrometry (LC-MS/MS) for the first time. The analyte and internal standard (IS), oleanic acid, were extracted from plasma with methanol and chromatographied on a C18 short column eluted with a mobile phase of methanol–water–formic acid (95:5:0.1, v/v/v). Detection was performed by positive ion atmospheric pressure chemical ionization in selective reaction monitoring mode. This method monitored the transitions m/z 409.0 →109.2 and m/z 439.4 → 203.2 for euphol and IS, respectively. The assay was linear over the concentration range 27–9000 ng/mL, with a limit of quantitation of 27 ng/mL. The accuracy was between –7.04 and 4.11%, and the precision was <10.83%. This LC-MS/MS method was successfully applied to investigate the pharmacokinetic study of euphol in rats after intravenous (6 mg/kg) and oral (48 mg/kg) administration. Results showed that the absolute bioavailability of euphol was approximately 46.01%.
大戟醇是从甘遂中分离出的一种具有潜在药理活性的成分。首次基于液相色谱-串联质谱法(LC-MS/MS)开发了一种简单、快速且灵敏的测定大鼠血浆中大戟醇的方法。分析物和内标(IS)齐墩果酸用甲醇从血浆中提取,并在C18短柱上进行色谱分离,流动相为甲醇-水-甲酸(95:5:0.1,v/v/v)。采用正离子大气压化学电离在选择性反应监测模式下进行检测。该方法分别监测大戟醇和内标的m/z 409.0→109.2和m/z 439.4→203.2的跃迁。该测定在27–9000 ng/mL的浓度范围内呈线性,定量限为27 ng/mL。准确度在–7.04%至4.11%之间,精密度<10.83%。该LC-MS/MS方法成功应用于研究大戟醇在大鼠静脉注射(6 mg/kg)和口服(48 mg/kg)给药后的药代动力学研究。结果表明,大戟醇的绝对生物利用度约为46.01%。