Zhao Xu, Ma Tiancheng, Zhang Chenning, Shi Shaohuai, Cui Sijiao, Bi Kaishun, Jia Ying
Shenyang Key Laboratory of Active Components of Chinese Medicine Screening and Evaluation, School of Traditional Chinese Materia Medica, Shenyang Pharmaceutical University, Wenhua Road 103, Shenyang, 110016, China.
The Engineering Laboratory of National and Local Union of Quality Control for Traditional Chinese Medicine, School of Pharmacy, Shenyang Pharmaceutical University, Wenhua Road 103, Shenyang, 110016, China.
Biomed Chromatogr. 2015 Sep;29(9):1297-303. doi: 10.1002/bmc.3420. Epub 2015 Jan 26.
A selective liquid chromatographic-mass spectrometric method has been developed and validated for simultaneous determination of senkyunolide I (SEI) and senkyunolide H (SEH) from Chuanxiong Rhizoma in rat plasma. Plasma samples were extracted by liquid-liquid extraction with ethyl acetate and separated on a Kromasil C18 column (250 × 4.6 mm, 5 µm), with methanol-water (55:45, v/v) as mobile phase. The linear range was 0.05-25 µg/mL for SEI and 0.01-5.0 µg/mL for SEH, with lower limits of quantitation of 0.05 and 0.01 µg/mL, respectively. Intra- and inter-day precision were within 10.0 and 9.8%, and the accuracies (relative errors) were <9.6 and 5.9%, with the mean extraction recoveries 81.0-86.6 and 80.5-85.0% for the two anayltes, respectively. The validated method was successfully applied to a comparative pharmacokinetic study of SEI and SEH in normal and migrainous rats after oral administration of Chuanxiong Rhizoma extract. The results indicated that there were obvious differences between normal and migrainous rats in the pharmacokinetic behavior after oral administration of Chuanxiong Rhizoma extract. The absorption of SEI and SEH were significantly increased in migrainous rats compared with normal rats.
已开发并验证了一种选择性液相色谱 - 质谱法，用于同时测定大鼠血浆中川芎中的藁本内酯I（SEI）和藁本内酯H（SEH）。血浆样品通过乙酸乙酯液 - 液萃取进行提取，并在Kromasil C18柱（250×4.6 mm，5 µm）上分离，以甲醇 - 水（55:45，v/v）作为流动相。SEI的线性范围为0.05 - 25 µg/mL，SEH的线性范围为0.01 - 5.0 µg/mL，定量下限分别为0.05和0.01 µg/mL。日内和日间精密度分别在10.0%和9.8%以内，准确度（相对误差）分别<9.6%和5.9%，两种分析物的平均提取回收率分别为81.0 - 86.6%和80.5 - 85.0%。该验证方法成功应用于口服川芎提取物后正常大鼠和偏头痛大鼠中SEI和SEH的比较药代动力学研究。结果表明，口服川芎提取物后，正常大鼠和偏头痛大鼠的药代动力学行为存在明显差异。与正常大鼠相比，偏头痛大鼠中SEI和SEH的吸收显著增加。
