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作 者:范荣[1,2] 黄熙[1,2] 王杨[1,2] 任平[1,2] 秦锋[1,2] 张春虎[1,2] 范岚[3,2] 高利臣[3,2] 刘昭前[3,2] 周宏灏[3,2]
机构地区:[1]中南大学湘雅医院中西医结合科国家中医药管理局肝藏象重点研究室 [2]中南大学中药遗传药理研究室,长沙410008 [3]中南大学临床药理研究所
出 处:《世界科学技术-中医药现代化》2011年第4期676-680,共5页Modernization of Traditional Chinese Medicine and Materia Medica-World Science and Technology
基 金:国家中医药管理局肝藏象重点研究室经费资助,负责人:黄熙;国家自然科学基金(81072967):从脑肠轴异常-肝郁脾虚途径研究逍遥散抗抑郁促胃肠动力的分子机制,负责人:任平,国家自然科学基金(30572339):丹参与柴胡复方质量控制成分的药理学基础,负责人:黄熙;湖南省中医药科研计划项目(2010113):中药复方丹川红抗氧化脑保护作用的机理研究,负责人:范荣
摘 要: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.
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