【作者】 龚红全；

【导师】 毋福海；

【作者基本信息】 广东药学院 ， 药物化学， 2008， 硕士

【摘要】 全文共分五个部分,主要内容和方法如下:第一章介绍了毛细管电泳在中药分析中的应用和发展,阐述了本课题的研究背景和意义。第二章建立同时测定白芷及其制剂元胡止痛片中欧前胡素和异欧前胡素含量的方法。采用非水胶束电动色谱法。电泳条件:采用未涂层弹性融硅石英毛细管柱(55cm×75μm ID,有效长度47cm);以20mmol/LNaH2PO4+100mmol/LSDS+80%甲酰胺溶液(pH7.12)为运行缓冲液;分离电压15kV;重力进样5s(高度15cm);检测波长254nm。以盐酸小檗碱为内标,欧前胡素、异欧前胡素的线性范围分别为8.0～40.0μg·ml?1(r=0.9987)、4.0～20.0μg·ml?1(r=0.9990);白芷中欧前胡素的平均回收率为100.1%,方法精密度(RSD)为2.83%(n=6);异欧前胡素平均回收率为102.4%,方法精密度(RSD)为3.07%(n=6)。;元胡止痛片中欧前胡素的平均回收率为101.3%,方法精密度(RSD)为2.58%(n=6);异欧前胡素平均回收率为100.2%,方法精密度(RSD)为2.64%(n=6)。该法简便、快速、准确可靠,可用于白芷及元胡止痛片的质量控制。第三章建立同时测定拈痛丸中盐酸小檗碱、盐酸巴马汀、盐酸药根碱、延胡索乙素含量的方法。采用毛细管电泳法。电泳条件:未涂层弹性融硅石英毛细管柱(55cm×75μm ID,有效长度47cm);以100 mmol/L磷酸二氢钠溶液+50%乙醇(pH5.70)为运行缓冲液;分离电压21kV;重力进样5s(高度15cm);检测波长211nm。以盐酸麻黄碱为内标,盐酸小檗碱、盐酸巴马汀、盐酸药根碱、延胡索乙素的线性范围分别为8.0～64.0μg·ml?1(r=0.9989)、2.5～12.5μg·ml?1(r=0.9997)、0.4～3.2μg·ml?1(r=0.9982)、0.2～1.6μg·ml?1(r=0.9987);拈痛丸中盐酸小檗碱的平均回收率为103.5%,方法精密度(RSD)为2.35%(n=6);盐酸巴马汀平均回收率为100.2%,方法精密度(RSD)为3.07%(n=6);盐酸药根碱平均回收率为102.8%,方法精密度(RSD)为3.10%(n=6);延胡索乙素平均回收率为97.8%,方法精密度(RSD)为2.71%(n=6)。该法简便、快速、准确可靠,可用于拈痛丸的质量控制研究。第四章建立了同时测定银黄胶囊及银黄颗粒中黄芩苷和绿原酸含量的方法。采用毛细管电泳法。电泳条件:未涂层弹性融硅石英毛细管柱(55cm×75μm ID,有效长度47cm);以40mmol/L硼砂溶液(pH9.30)为运行缓冲液;分离电压15kV;重力进样5s(高度15cm);检测波长310nm。以对硝基苯甲酸为内标,黄芩苷、绿原酸的线性范围分别为20.2～101.0μg·ml?1(r=0.9981),5.15～25.75μg·ml?1(r=0.9991)。银黄胶囊中黄芩苷、绿原酸的平均回收率分别为105.0%、97.2%,银黄颗粒中黄芩苷、绿原酸的平均回收率分别为101.3%、96.6%。该法简便、快速、准确可靠,可用于银黄胶囊及银黄颗粒的质量控制。第五章建立同时测定银黄胶囊中黄芩素、汉黄芩苷、汉黄芩素、绿原酸含量的方法。采用毛细管电泳法。电泳条件:采用未涂层弹性融硅石英毛细管柱(55cm×75μm ID,有效长度47cm);以40mmol/L硼砂溶液+15mmol/Lβ-环糊精(pH9.35)为运行缓冲液;分离电压12kV;重力进样5s(高度15cm);检测波长280nm。以对氨基苯甲酸为内标,黄芩素、汉黄芩苷、汉黄芩素、绿原酸的线性范围分别为2.5～12.5μg·ml?1(r=0.9986)、10.0～80.0μg·ml?1(r=0.9981)、1.25～10.0μg·ml?1(r=0.9995)、15.0～120.0μg·ml?1(r=0.9984);银黄胶囊中黄芩素的平均回收率为104.6%,方法精密度(RSD)为2.57%(n=6);汉黄芩苷平均回收率为97.2%,方法精密度(RSD)为1.97%(n=6);汉黄芩素平均回收率为98.5%,方法精密度(RSD)为2.87%(n=6);绿原酸平均回收率为95.8%,方法精密度(RSD)为2.88%(n=6)。该法简便、快速、准确可靠,可用于银黄胶囊的质量控制研究。更多还原

【Abstract】 This thesis includes the following five chapters:Chapter 1We introduced the application and development of capillary electrophoresis in the analysis of traditional chinese medicine,narrated the background and significance of our study.Chapter 2To establish a method for the determination of imperatorin and isoimperatorin in Radix Angelicae dahuricae and Yuanhu Zhitong Pian by non-aqueous micelle using capillary electrokinetic chromatography. The separation was performed on a uncoated fused silica capillary of 55cm×75μm ID (47cm effective length). 20mmol/L NaH2PO4 +100 mmol/LSDS+80%formamide buffer solution(pH7.12) was selected for the running buffer. The voltage applied was 15kV. The sample was injected by gravity(5s,15cm). The detection wavelength was 254 nm. The internal standard was berberine hydrochloride. The linear ranges of determination for imperatorin and isoimperatorin were 8.0～40.0μg·ml?1(r=0.9987)and 4.0～20.0μg·ml?1(r=0.9990). The average recovery for imperatorin in Radix Angelicae dahuricae was 100.1%,precision of the method was 2.83%(RSD,n=6). The average recovery for isoimperatorin in Radix Angelicae dahuricae was 102.4%,precision of the method was 3.07%(RSD,n=6). The average recovery for imperatorin in Yuanhu Zhitong Pian was101.3%,precision of the method was 2.58%(RSD,n=6). The average recovery for isoimperatorin in Yuanhu Zhitong Pian was 100.2%,precision of the method was 2.64%(RSD,n=6). The method proved to be conveient、rapid and well repeatable,and can be used for quantitative determination of Radix Angelicae dahuricae and Yuanhu Zhitong Pian.Chapter 3To establish a method for the determination of berberine hydrochloride、palmatine hydrochloride、jatrorrhizine hydrochloride and tetrahydropalmatine in Niantong Wan by capillary electrophoresis. The separation was performed on a uncoated fused silica capillary of 55cm×75μm ID ( 47cm effective length ) . 100 mmol/L sodium dihydrogen phosphate+50% ethano(lpH5.70) was selected for the running buffer. The voltage applied was 21kV. The sample was injected by gravity(5s,15cm). The detection wavelength was 211 nm. The linear ranges of determination for berberine hydrochloride、palmatine hydrochloride、jatrorrhizine hydrochloride and tetrahydropalmatine were 8.0～64.0μg·ml?1(r=0.9989)、2.5～12.5μg·ml?1(r=0.9997)、0.4～3.2μg·ml?1(r=0.9982)、0.2～1.6μg·ml?1(r=0.9987). The average recovery for berberine hydrochloride was 103.5%,precision of the method was 2.35% (RSD,n=6). The average recovery for palmatine hydrochloride was 100.2%,precision of the method was 3.07% (RSD,n=6). The average recovery for jatrorrhizine hydrochloride was 102.8%,precision of the method was 3.10% (RSD,n=6). The average recovery for tetrahydropalmatine was 97.8%,precision of the method was 2.71% (RSD,n=6). The method proved to be conveient、rapid and well repeatable,and can be used for quantitative determination of the preparation.Chapter 4To establish a method for the determination of baicalin and chlorogenic acid in Yinhuang Jiaonang and Yinhuang Keli by capillary electrophoresis. The separation was performed on a uncoated fused silica capillary of 55cm×75μm ID (47cm effective length). 40 mmol/L Na2B4O7 buffer solution(pH9.30) was selected for the running buffer. The voltage applied was 15kV. The sample was injected by gravity(5s,15cm). The detection wavelength was 310 nm. The linear ranges of determination for baicalin and chlorogenic acid were 20.2～101μg·ml?(1r=0.9981) and 5.15～25.75μg·ml?(1r=0.9991). The average recoveries of baicalin and chlorogenic acid were 105.0% and 97.2% in Yinhuang Jiaonang,respectively. The average recoveries of baicalin and chlorogenic acid were 101.3% and 96.6% in Yinhuang Keli,respectively. The method proved to be conveient、rapid and well repeatable,and can be used for quantitative determination of the preparation.Chapter 5To establish a method for the determination of baicalein、wogonoside、wogonin and chlorogenic acid in Yinhuang Jiaonang by capillary electrophoresis. The separation was performed on a uncoated fused silica capillary of 55cm×75μm ID (47cm effective length). 40 mmol/L Na2B4O7 + 15 mmol/Lβ-CD buffer solution(pH9.35) was selected for the running buffer. The voltage applied was 12kV. The sample was injected by gravity(5s,15cm). The detection wavelength was 280 nm. The linear ranges of determination for baicalein、wogonoside、wogonin and chlorogenic acid were 2.5～12.5μg·ml?1(r=0.9986)、10.0～80.0μg·ml?(1r=0.9981)、1.25～10.0μg·ml?(1r=0.9995)、and 15.0～120.0μg·ml?1(r=0.9984). The average recovery for baicalein was 104.6%,precision of the method was 2.57% (RSD,n=6). The average recovery for wogonoside was 97.2%,precision of the method was 1.97% (RSD,n=6). The average recovery for wogonin was 98.5%,precision of the method was 2.87% (RSD,n=6). The average recovery for chlorogenic acid was 95.8%,precision of the method was 2.88% (RSD,n=6). The method proved to be conveient、rapid and well repeatable,and can be used for quantitative determination of the preparation.更多还原