UPLC法测定脑外伤患者口服大黄吸收入血蒽醌类成分

Determination of Anthraquinones in Traumatic Cerebral Injury Patient after Oral Administration of Rhubarb by UPLC Method

目的：建立超高效液相色谱（UPLC）法测定口服大黄脑外伤患者血浆中蒽醌类成分。方法：采用Waters Acquity UPLC BEH C18（2．1mm×100mm，1．7μm）色谱柱，以甲醇-0．5％醋酸（12：82）为流动相，检测波长：254nm，流速：0．5mL·min-1，柱温：25℃，进样量：5μL。结果：大黄酸的血浆中浓度分别在0．42～13．429μg·min-1内线性范围良好，其他4种蒽醌类成分未被检测出，方法回收率在97．2％～103．11％之间，日内、日间RSD均小于6％；本法检测出5名重型脑外伤病人1h血浆样品中大黄酸的质量浓度为7．93＋1．94μg·min-1。结论：本法精密度好，回收率高，操作简便、无毒、重现性好。

Ultra-performance liquid chromatography （UPLC）method was developed for determination of anthraquinones in plasma of patient with traumatic brain injury （TBI） after Rhubarb administration. Chromatographic separation was performed on an Acquity UPLC BEH C18 column （2.1mm×100mm, 1.7μm） with methanol-0.5% aqueous acetic acid （12：82） as mobile phase at a flow rate of 0.5mL ·min-1. The wavelength was set at 254nm. The operating temperature was maintained at 25℃ and the sample volume injected was 5μL. Linear range was satisfactory for determination of rhein in human plasma with the concentration range from 0.42μg·mL-L to 13.429μg·mL-L Other four anthraquinones were not detected with UPLC method. Recovery rate of this method was within the range of 97.2%-103.11%. The relative standard deviation of intra- and inter-day was less than 6%. The concentration of rhein in plasma after one hour administration form five TBI patients was 7.93±1.94μg·mL-L. The UPLC is a method with good precision, high recovery rate, simple operation, innocuity and good reproducibility.