Biomedicine Key Laboratory of Shaanxi Province, The School of Life Sciences, Northwest University, Xi'an, Shaanxi 710069, China.
J Chromatogr B Analyt Technol Biomed Life Sci. 2011 Jul 1;879(21):1945-53. doi: 10.1016/j.jchromb.2011.05.025. Epub 2011 May 23.
Rapid resolution liquid chromatography/tandem multi-stage mass spectrometry (RRLC-MS(n)) and rapid resolution liquid chromatography/tandem mass spectrometry (RRLC/MS/MS) methods were developed for the identification and quantification of ergosterol and its metabolites from rat plasma, urine and faeces. Two metabolites (ERG1 and ERG2) were identified by RRLC/MS(n). The concentrations of the ergosterol were determined by RRLC/MS/MS. The separation was performed on an Agilent Zorbax SB-C18 with the mobile phase consisting of methanol and water (containing 0.1% formic acid). The detection was carried out by means of atmospheric pressure chemical ionization mass spectrometry in positive ion mode with multiple reaction monitoring (MRM). Linear calibration curves were obtained in the concentration range of 7-2000, 6-2000 and 8-7500 ng/mL for plasma, urine and faecal homogenate, respectively. The intra- and inter-day precision values (RSD) were below 10%. The method was applied to the pharmacokinetic properties and elimination pathway of ergosterol in rats.
建立了用于鉴定和定量大鼠血浆、尿液和粪便中麦角甾醇及其代谢物的快速分辨液相色谱/串联多级质谱(RRLC-MS(n))和快速分辨液相色谱/串联质谱(RRLC/MS/MS)方法。通过 RRLC/MS(n) 鉴定出 2 种代谢物(ERG1 和 ERG2)。采用 RRLC/MS/MS 测定麦角甾醇的浓度。分离在 Agilent Zorbax SB-C18 上进行,流动相由甲醇和水(含 0.1%甲酸)组成。检测采用正离子模式大气压化学电离质谱,多反应监测(MRM)。在血浆、尿液和粪便匀浆中的浓度范围分别为 7-2000、6-2000 和 8-7500 ng/mL 时,得到了线性校准曲线。日内和日间精密度(RSD)均低于 10%。该方法应用于大鼠麦角甾醇的药代动力学特性和消除途径。