【作者】 邹欢；

【导师】 贺福元；

【作者基本信息】 湖南中医药大学 ， 中药学， 2010， 硕士

【摘要】 目的：本文以补阳还五汤为模型药物,通过对此方中总苷类有效成分群提取动力学,溶度峰及介电需量,大孔吸附树脂柱层析行为的研究,探索补阳还五汤总苷类有效成分群在提取分离过程中的动态迁移规律,为实现中药复方有效成分群的定位定量提取分离提供实验依据。方法：1.建立了补阳还五汤总苷类有效成分群的含量测定方法-差示蒽酮-糖脎显色法及补阳还五汤总苷类有效成分群的指纹图谱；2.结合补阳还五汤总苷类有效成分群的含量测定方法,对不同提取时间的原方总苷类有效成分群的含量进行多元非线性参数估算,根据已建立的数学模型计算出其提取动力学参数；3.根据介电常数理论测定补阳还五汤总苷类有效成分群的溶度峰和介电需量,获得最佳提取分离溶媒；4.依据柱层析色谱理论,利用最佳的提取分离溶媒,测算得到补阳还五汤总苷类有效成分群在大孔树脂层析分离时的最佳流速,以及层析分离工艺参数,从而得到有效成分群用量/固定相量/洗脱剂溶度参数三者的关系结果：1.首次建立了中药复方总苷类成分的含量测定方法—差式蒽酮-糖脎比色法；2.补阳还五汤中总苷类有效成分群的提取动力学药时曲线呈三室模型(R>0.94),主要提取动力学参数tmax,cmax,P,D分别为128.9min,38.17%,38.16%,24.45%；3.补阳还五汤总苷类有效成分群的介电需量为51.6,最佳的提取分离溶媒为50%乙醇溶液；4.补阳还五汤总苷类有效成分群在大孔吸附树脂柱层析分离时的最佳流速为2.02 cm/min,主要色谱参数Cm,Cs,吸附平衡常数K及容量因子k分别为28.38 mg·mL-1,95.38 mg·mL-1,3.360,8.213;当树脂用量为30mL时的理论塔板高度最小,柱效最好,此时总苷类有效成分群的保留体积为80mL,理论塔板高度和理论塔板数分别为0.3662,40.96。结论：差式蒽酮-糖脎比色法适合于总苷类成分的含量测定；中药复方提取动力学数学模型能客观地描述中药复方中有效成分群的提取行为,是研究中药复方溶解规律和提取工艺的有效工具；补阳还五汤总苷类有效成分群在进行大孔吸附树脂层析分离时,外部条件一定的情况下,可以通过控制其流速,控制有效成分群的量、固定相的用量、流动相的溶度参数,实现补阳还五汤总苷类有效成分群的定位定量分离。更多还原

【Abstract】 Objection:To clarify the dissolution and transfer rule during the extraction and separation process by detecting the extraction kinetical profile, the solubility peak and dielectric requirement and the column chromatography behavior of macroreticular Resin for glycosides effective component groups of BYHWD,and supply experimental foundation for the orientation and quantification fractionation of the effective component group of the Chinese Medicine Compound Prescription.Method:1.Methods for the content determination and the fingerprint of glycosides effective component group was establishen, which is the differential anthrone-glucose phenylosazone colorimetric method(DAGC);2.By the method of content determination of the glycosides effective component group of BYHWD and the established kinetics model,the kinetical profile deviations and the extraction kinetical curve of glycosides effective component group of BYHWD were carried out; 3.According to the theory of dielectric constants the Solubility peak and dielectric requirement of glycosides effective component group of BYHWD were detected, then the optimal solvent for fractionation of glycosides efficient components was obtained;4.By the column chromatography theory, the optimal velocity and the process parameters for the column chromatography separation behavior of the glycosides effective component group were determined using the optimal mobile phase,and getted the relationship among the quantity of glycosides effective component group of BYHWD, of the stationary phase and the solubility parameter of mobile phaseδm.Result:1.Firstly build the content determination method for glycosides component of the Chinese Medicine Compound Prescription;2.The extraction kinetical profiles for the the glycosides effective component group were fitted three compartment model (R>0.94); The main kinetical parameters tmax,cmax,P,D of the glycosides effective component group of BYHWD were respectively 128.9min,38.17%, 38.16%,24.45%;3.The dielectric requirement of glycosides effective component group of BYHWD was 51.6, and the optimal solvent for fractionation of glycosides efficient components was 50% ethanol solution;4.the optimal velocity for the column chromatography separation behavior of the glycosides effective component group was 2.02 cm/min, and the main process parametersCm Cs K, k were 28.38 mg·mL-1,95.38 mg·mL-1,3.360,8.213 respectively; when the volume of resin was 30 mL, the retention volume of glycosides effective component group of BYHWD was 80 mL with the best column efficiency,and the theory Plate Count and the plate height respectively were 0.3662,40.96.Conclution:It was been validated that the DAGC method was a useful method for the content determination of the glycosides effective component group of BYHWD;It is suggested that for the effective component group of the Chinese Medicine Compound Prescription, the extraction kinetics model was decribed objectively the extraction kinetical profiles, which was a useful tool to study their solubility rules and extraction technique;as the column, the temperature and the stationary phase are all invariable, the orientation and quantification fractionation process for the glycosides effective component group of BYHWD can be carried out by control the velocity, the sample size, the quantity of stationary phase and the solubility parameter of mobile phase δm.更多还原