柴胡疏肝汤高效液相指纹图谱及其含量测定研究

发布时间：2018-03-10 11:07

本文选题：柴胡疏肝汤　切入点：高效液相色谱　出处：《南方医科大学》2017年硕士论文　论文类型：学位论文

【摘要】：背景与目的柴胡疏肝汤是本课题组根据癫痫“从肝论治”治疗理论组建的复方,由柴胡、黄芩、白芍等15味中药组成,具有疏肝、柔肝、养肝、平肝作用,现代研究表明,此方具有降低神经兴奋性、抗炎和调节机体免疫功能的作用。该方为附属医院中药房的协定处方,已在临床运用30余年,在癫痫预防和治疗上取得了确切疗效。中药质量的好坏与临床用药疗效及安全密切相关。目前柴胡疏肝汤尚未有相关质量控制研究,本文将采用高效液相色谱法对柴胡疏肝汤进行系统研究,建立柴胡疏肝汤指纹图谱,并对其主要成分含量进行测定,从整体和部分有效成分上对其质量进行全面控制,为临床用药安全及该方进一步研究提供理论依据。方法1.柴胡疏肝汤高效液相指纹图谱研究及其主要成分黄芩苷、汉黄芩苷、汉黄芩素、芍药苷、阿魏酸、甘草苷的含量测定。采用高效液相色谱法,二极阵列检测器,Agilent ZORBAX SB-C8色谱柱(250 mm×4.6mm,5μm),在检测波长210nm、柱温25℃下,进样量为10μL,以乙腈(A)-0.2%磷酸水溶液(B)为流动相进行梯度洗脱,检测时间为65 min。测定10批柴胡疏肝汤色谱图,评估柴胡疏肝汤整体质量的相似度,分析该方共有特征峰药物归属。在相同的色谱条件下,建立其多成分含量测定方法,为柴胡疏肝汤的质量控制提供依据。2.柴胡疏肝汤主要成分柴胡皂苷a、汉黄芩苷、芍药苷的含量测定。采用高效液相色谱法,二极阵列检测器,Agilent ZORBAX SB-C8色谱柱(250 mmx4.6mm,5 μm),在检测波长210nm、柱温25℃C下,进样量为10μL,以乙腈(A)-0.2%磷酸水溶液(B)为流动相进行梯度洗脱,检测时间为80 min。考察了柴胡皂苷a、汉黄芩苷、芍药苷的稳定性、重复性,测定其含量,为该方质量控制提供依据。结果1.建立了柴胡疏肝汤高效液相指纹图谱,10批样品的相似度较好均大于0.95。确定共有峰有22个,明确各峰所归属药材,其中7个色谱峰可明确化学成分。同时建立了能同时测定柴胡疏肝汤中主要成分芍药苷、黄芩苷、汉黄芩苷、汉黄芩素、阿魏酸、甘草苷含量方法。线性关系良好,平均加样回收率(n=9)均在 90～105%(RSD3%)。2.建立测定柴胡疏肝汤中主要成分柴胡皂苷a、汉黄芩苷、芍药苷的含量方法,在24小时内稳定,重复性可,线性关系良好,平均加样回收率(n=9)均在90～105%(RSD3%)。结论建立柴胡疏肝汤高效液相指纹图谱及含量测定方法,该方法重复性、稳定性可,线性关系、平均加样回收率良好,可以反映柴胡疏肝汤整体特性。为柴胡疏肝汤质量控制及进一步研究提供理论基础。
[Abstract]:Background and objective: ChaiHuShuGan decoction is the research group according to the epilepsy "from the liver" therapy theory established by compound, bupleurum, Scutellaria, Radix Paeoniae Alba composed of 15 herbs, with soothing liver, nourishing liver, liver function, modern research shows that this has reduced nerve excitability, anti-inflammatory and immune regulation function of body. The agreement prescription for Affiliated Hospital Pharmacy in more than 30 years, has been used in clinical, has exact curative effect in the prevention and treatment of epilepsy. Traditional Chinese medicine quality and clinical efficacy and safety are closely related. At present there is no Tangshang Chai Hushu liver related research quality control, this paper will use the high performance liquid chromatography chromatography system research of ChaiHuShuGan Decoction ChaiHuShuGan decoction, establishment of fingerprint, and its main components were determined, to conduct a comprehensive control of its quality from the whole and part of effective components, for clinical use Drug safety and the further research and provide a theoretical basis for the study. Map and its main component baicalin method 1. chaihushugantang HPLC fingerprint, baicalin, wogonin, paeoniflorin, ferulic acid, determination of liquiritin. By HPLC diode array detector, Agilent ZORBAX SB-C8 chromatography column (250 mm * 4.6mm, 5 m), at the detection wavelength of 210nm, the column temperature of 25 DEG C, the injection volume was 10 L (A), acetonitrile -0.2% phosphoric acid solution (B) as the mobile phase with gradient elution. The detection time is 65 min. by the 10 batch of chaihushugantang chromatograms. The similarity of overall quality assessment of ChaiHuShuGan decoction, analysis the common characteristic peaks of drugs belonging. Under the same chromatographic conditions, to establish a method for determination of the content, for the quality control of ChaiHuShuGan Decoction ChaiHuShuGan Decoction.2. provide the basis for the main components of saikosaponin a, baicalin, paeoniflorin The content determination by high performance liquid chromatography diode array detector, Agilent ZORBAX SB-C8 column (250 mmx4.6mm, 5 m), at the detection wavelength of 210nm, the column temperature 25 DEG C, the injection volume was 10 L (A), acetonitrile -0.2% phosphoric acid solution (B) as mobile phase. Gradient elution, detection time is 80 min. The effects of saikosaponin a, baicalin, paeoniflorin, stability, repeatability, determination of its content, provide the basis for the quality control. Results 1. established chaihushugantang HPLC fingerprints of 10 batches of samples of high similarity were more than 0.95. were determined there are 22 clear peaks, each peak belongs to medicine, among which 7 peaks can clear the chemical composition. At the same time to establish a simultaneous determination of paeoniflorin ingredient of ChaiHuShuGan Decoction in glycosides, baicalin, wogonoside, wogonin, ferulic acid, liquiritin. Method of linear relationship, the average sample the recovery rate (n=9 ) were in the range of 90 to 105% (RSD3%).2. determination of ChaiHuShuGan Decoction in main ingredients saikosaponin a, baicalin, paeoniflorin content method, stable in 24 hours, repeatability, good linear relationship, the average recovery rate (n=9) were in the range of 90 to 105% (RSD3%) conclusion. The establishment of chaihushugantang HPLC fingerprint and determination, the method repeatability, stability, linear relationship, the average recovery rate is good, can reflect the overall characteristics of ChaiHuShuGan decoction. It provides the theoretical basis for the quality control of ChaiHuShuGan Decoction and further study.

【学位授予单位】：南方医科大学
【学位级别】：硕士
【学位授予年份】：2017
【分类号】：R286.0;O657.72

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