【作者】 李丹；

【导师】 赵春杰；

【作者基本信息】 沈阳药科大学 ， 药物分析学， 2008， 硕士

【摘要】 血府逐瘀丸是清·王清仁《医林改错》的改良新产品,是由桃仁、红花、当归、赤芍、生地黄、川芎、牛膝、桔梗、柴胡、枳壳、甘草十一味药材组成的复方中药,本文对其提取工艺、质量评价方法及金属元素进行了研究。以甲醇回流提取法,采用正交试验设计,选取羟基红花黄色素A、阿魏酸、芍药苷、橙皮苷的含量四个考察指标,对提取工艺中甲醇用量、提取时间和提取次数三个因素进行优化。通过综合评价法确定最优工艺为:用20倍量的甲醇,水浴回流一次,每次1h。建立了同时测定血府逐瘀丸中有效成分羟基红花黄色素A、阿魏酸、芍药苷、橙皮苷含量的反相高效液相色谱分析方法,采用Kromasil ODS色谱柱（250 mm×4.6 mm,5μm）,以乙腈-0.25%冰醋酸水溶液进行线性梯度洗脱,流速为1.0 mL·min^-1,检测波长265 nm,进样量20μL。实验结果表明:羟基红花黄色素A在23.85～119.3μg·mL^-1范围内线性关系良好,相关系数为0.9996,平均回收率为99.8%,RSD为1.4%;芍药苷在140～644μg·mL^-1范围内线性关系良好,相关系数为0.9992,平均回收率为100.3%,RSD为0.3%;阿魏酸在10.25～47.15μg·mL^-1范围内线性关系良好,相关系数为0.9993,平均回收率为96.6%,RSD为2.0%;橙皮苷在130-598μg·mL^-1范围内线性关系良好,相关系数为1.0,平均回收率为100.4%,RSI)为1.0%。该方法准确、重复性好,为评价血府逐瘀丸质量提供了一种定量依据。同时对处方中当归、赤芍、枳壳进行了薄层色谱定性分析。本研究建立的定性、定量分析方法能更加全面地控制该方的质量,并且优化后的提取工艺可为今后剂型的改进提供基础。同时建立了测定血府逐瘀丸中钙、镁、锌、铜、铁、锰、镍、铬八种元素的火焰原子吸收分光光度法,采用硝酸-高氯酸（4:1,v/v）常压微沸条件下消解样品。实验结果表明,钙在1.0～8.0μg·mL^-1范围内线性关系良好,相关系数为0.9994,平均回收率为100.2%,RSD为1.5%;镁在0.1～3.0μg·mL^-1范围内线性关系良好,相关系数为0.9995,平均回收率为98.4%,RSD为2.7%;锌在0.3～2.0μg·mL^-1范围内线性关系良好,相关系数为0.9995,平均回收率为104.5%,RSD为4.4%;铜在0.1～0.5μg·mL^-1范围内线性关系良好,相关系数为0.9993,平均回收率为101.8%,RSD为2.3%;铁在0.5～6.0μg·mL^-1范围内线性关系良好,相关系数为1.0,平均回收率为101.5%,RSD为3.0%;锰在0.1～1.6μg·mL^-1范围内线性关系良好,相关系数为0.9996,平均回收率为103.9%,RSD为3.2%;镍在0.1～0.5μg·mL^-1范围内线性关系良好,相关系数为0.9992,平均回收率为104.7%,RSD为4.5%;铬在0.05～0.4μg·mL^-1范围内线性关系良好,相关系数为1.0,平均回收率为102.3%,RSD为2.3%。该方法准确、迅速、简便,为血府逐瘀丸质量评价提供了另一种定量依据,为今后进一步研究宏量微量元素与疾病的发生发展密切相关提供基础。更多还原

【Abstract】 Xuefuzhuyu pill was reported originally in yilingaicuo,written by Wang Qingren.This paper is about the extraction process and quality assessment and the study of constant & metal elements,which is composed of Semen Persicae、Flos Carthami、Radix Angelicae Sinensis、Radix Rehmanniae、Rhizoma Chuanxiong、Radix Paeoniae Rubra、Radix Achyranthis Bidentatae、Radix Platycodi、Radix Bupleuri、Fructus Aurantii and Radix Glycyrrhizae.The optimal alcohol extraction process of Xuefuzhuyu pill was studied by orthogonal design with extractive yield and the contents of hydro-saffior yellow A,paeoniflorin,ferulic acid and hesperidin from Xuefuzhuyu pill as quality assessment indices.Three factors were studied in this experiment,including the methanol consumption,duration of extration and times of extration.The results showed that the optimal extraction condition was methanol consumpted 20 times the amount of material,refluxing for once and 1 hour per time.RP-HPLC methods were established to simultaneously determine hydro-saffior yellow A in Carthamus tinctorius L.,paeoniflorin in Radix Paeoniae Alba,ferulic acid in Radix Angelicae Sinensis and Radix Ligusticum wallichii Franch.,hesperidin in Poncirus trifoliata （L.）Rafi and Citrus aurantium L..The separatior of four marker compounds was achieved on a Kromasil C₁₈column（250 mmx4.6 mm,5μm）with gradient elution using solvents of acetonitrile and aqueous acetic acid.The detection wavelength was set at 265 nm and the flow rate was 1.0 mL·min^-1.Assay was linear over the range 23.85～119.3μg·mL^-1for hydro-safflor yellow A（r=0.9996）,140～644μg·mL^-1for paeoniflorin（r=0.9992）,10.25～47.15μg·mL^-1for ferulic acid（r=0.9993）,130～598μg·mL^-1for hesperidin（r=1.0）. Average recoveries of samples were 99.8%（RSD=1.4%）,100.3%（RSD=0.3%）,96.6% （RSD=2.0%）and100.4%（RSD=1.0%）for four constituents,respectively.Three herbs of Xuefuzhuyu pill were indentified by TLC with the dots clear and reproducible.The assay methods were accurate and with good reproducibility and provided a quantitative basis for the quality assessment for Xuefuzhuyu pill.FAAS methods were also established to simultaneously determine Ca、Mg、Zn、Cu、Fe、Mn、Ni、Cr.The samples were digested with HNO₃-HCLO₄（4:1,v/v）at 140℃under normal pressure.Assay was linear over the range 23.85～119.3μg·mL^-1for hydro-safflor yellow A（r=0.9996）,1.0～8.0μg·mL^-1for Ca（r=0.9994）,0.1～3.0μg·mL^-1for Mg（r=0.9995）, 0.3～2.0μg·mL^-1for Zn（r=0.9995）,0.1～0.5μg·mL^-1for Cu（r=0.9993）,0.5～6.01μg·mL^-1for Fe（r=1.0）,0.1～1.6μg·mL^-1for Mn（r=0.9996）,0.1～0.5μg·mL^-1for Ni（r=0.9992）,0.05～0.4μg·mL^-1for Cr（r=1.0）.Average recoveries of samples were 100.2%（RSD =1.5%）, 98.4%（RSD=2.7%）,104.5%（RSD =4.4%）,101.8%（RSD =2.3%）,101.5%（RSD =3.0 %）,103.9%（RSD=3.2%）,104.7%（RSD=4.5%）and 102.3%（RSD=2.3%）for eight elements,respectively.The assay methods were accurate,rapid and simple,providing a quantitative basis for the quality assessment for Xuefuzhuyu pill in another way and providing a basis to study the relationship between elements and diseases.更多还原