Zhang Nan, Pang Li, Dong Ning, Xu Dahai, Xu Hong
Emergency Department, the First Hospital of Jilin University, Changchun, 130021, China.
Gastrointestinal Medicine, the First Hospital of Jilin University, Changchun, 130021, China.
Biomed Chromatogr. 2015 Nov;29(11):1643-9. doi: 10.1002/bmc.3473. Epub 2015 Apr 14.
Taraxasterol, a pentacyclic triterpene from Taraxacum officinale, is one of the main active constituents of the herb. This study developed and validated a highly selective and sensitive liquid chromatography/tandem mass spectrometry for the determination of taraxasterol in rat plasma over the range of 9.0-5000 ng/mL. Chromatographic separation was achieved on a C18 (4.6 × 50 mm, 5.0 µm) column with methanol-isopropanol-water-formic acid (80:10:10:0.1, v/v/v/v) as mobile phase with an isocratic elution. The flow rate was 0.7 mL/min. After adding cucurbitacin IIa as an internal standard (IS), liquid-liquid extraction was used for sample preparation using ethyl acetate. The atmospheric pressure chemical ionization source was applied and operated in positive ion mode. Selected reaction monitoring mode was used for the quantification of transition ions m/z 409.4 → 137.1 for taraxasterol and m/z 503.4 → 113.1 for IS. The mean recoveries of taraxasterol in rat plasma ranged from 85.3 to 87.2%. The matrix effects for taraxasterol were between 98.5 and 104.0%. Intra- and inter-day precision were both <11.8%, and the accuracy of the method ranged from -7.0 to 12.9%. The method was successfully applied to a pharmacokinetic study of taraxasterol after oral administration of 7.75, 15.5 and 31.0 mg/kg in rats.
蒲公英甾醇是一种来自药用蒲公英的五环三萜，是该草药的主要活性成分之一。本研究开发并验证了一种高选择性和灵敏的液相色谱/串联质谱法，用于测定大鼠血浆中浓度范围为9.0 - 5000 ng/mL的蒲公英甾醇。采用C18（4.6×50 mm，5.0 µm）色谱柱，以甲醇 - 异丙醇 - 水 - 甲酸（80:10:10:0.1，v/v/v/v）为流动相进行等度洗脱，实现色谱分离。流速为0.7 mL/min。加入葫芦素IIa作为内标后，采用乙酸乙酯进行液 - 液萃取制备样品。采用大气压化学电离源，以正离子模式运行。选择反应监测模式用于定量蒲公英甾醇的过渡离子m/z 409.4 → 137.1和内标的过渡离子m/z 503.4 → 113.1。大鼠血浆中蒲公英甾醇的平均回收率为85.3%至87.2%。蒲公英甾醇的基质效应在98.5%至104.0%之间。日内和日间精密度均<11.8%，该方法的准确度范围为 - 7.0%至12.9%。该方法成功应用于大鼠口服7.75、15.5和31.0 mg/kg蒲公英甾醇后的药代动力学研究。
