密闭微波辅助提取-HPLC测定中成药中黄芩苷及绿原酸的研究
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摘要
中成药是在中医药理论指导下,以中药材为原料,按照规定的处方、生产工艺和质量标准生产的制剂,具有便于携带、使用方便、毒副作用小等特点。随科学技术的发展,中医药学现代化也使中成药在人们疾病防治中大显身手,在各治疗领域发挥着重要作用。
黄芩苷和绿原酸存在于多种植物中,是许多中成药中药效成分。根据报道,黄芩苷和绿原酸均具有抗菌抗炎、消除自由基和抗氧化等作用。
本文针对银黄片和小儿清热宁颗粒中黄芩苷和绿原酸的微波辅助提取作了一系列的研究工作。
建立了采用微波辅助提取银黄片样品中绿原酸及黄芩苷、并以反相高效液相色谱法测定其含量的实验方法。分别通过单因素实验和正交实验设计,优化了萃取溶剂浓度、微波功率、微波辐射时间和微波提取温度四个提取条件,确定了微波辅助萃取法提取银黄片样品中的绿原酸及黄芩苷的最佳条件为:乙醇浓度70%,微波功率255W,提取时间1min,提取温度80℃。在上述最优条件下进行了精密度和回收率实验,绿原酸及黄芩苷加入回收率分别在96.2%～100.3%与96.5%～106.3%之间,RSD分别为3.69%(n=5)和4.03%(n=5)。
建立了采用微波辅助提取小儿清热宁颗粒样品中黄芩苷、并以反相高效液相色谱法测定其含量的实验方法。通过正交实验设计,优化了萃取溶剂浓度、微波功率、微波辐射时间和微波提取温度四个提取条件,确定了微波辅助萃取法提取小儿清热宁颗粒样品中的黄芩苷的最佳条件:提取溶剂为70%乙醇,微波功率为255W,微波提取时间为1min,提取温度为80℃。在上述最优条件下进行了精密度和回收率实验,黄芩苷加入回收率在96.9%～100.3%之间,RSD为2.42%(n=6)。与超声波提取法比较,微波辅助萃取法具有操作简便,快速,重现性好等特点。
通过以上两个体系的研究,可得出微波辅助提取-反相高效液相色谱法测定中成药中绿原酸及黄芩苷含量的方法稳定可靠,可为中成药中绿原酸及黄芩苷质量监控提供参考方法。
Traditional Chinese Medicine Patent Prescription(TCMPP) is a prescription which is produced in accordance with the provisions of the prescription,production processes and quality standards by Chinese herbal medicine under the guidence of Traditional Chinese Medicine(TCM) theory. TCMPP has many unique advantages,such as convenient to carry,easy to use, little toxicity and so on.With the modernization of TCM,TCMPP play more and more important role in the field of TCM.
Baicalin and Chlorogenic acid exist in many kinds of plants.They can be used as bioactive compounds in lots of TCMPP.It is reported that Baicalin and Chlorogenic acid have shown antibacterial,anti-inflammatory,significant scavenging of free oxygen radicals and antioxidative activity.
The microwave-assisted extraction of Baicalin and Chlorogenic acid of Yinhuang Tablets and Xiaoer Qingrening Granule was studied in this thesis.
Determination of Baicalin and Chlorogenic acid from Yinhuang Tablets by microwave-assisted extraction(MAE) and RP-HPLC was reported in the first part of thesis.The effects of solvent concentration,microwave power, extracting time and extracting temperature were evaluated by single factor and orthogonal experiments.The extraction conditions of Baicalin and Chlorogenic acid from Yinhuang Tablets by microwave-assisted method were optimized as follows:the ethanol concentration was 70%;the microwave power was 255 W;the extracting time was 1 min and extracting temperature was 80℃.Under the optimized conditions,the recovery of Baicalin and Chlorogenic acid were 96.2%～100.3%and 96.5%～106.3%,respectively.The relative standard deviation of Baicalin and Chlorogenic acid were 3.69%(n=5) and 4.03%(n=5),respectively.
Determination of Baicalin from Xiaoer Qingrening Granule by microwave-assisted extraction and RP-HPLC was reported in the second part of thesis.The effects of solvent concentration,microwave power,extracting time and extracting temperature were evaluated by orthogonal experiments. The extraction conditions of Baicalin from Xiaoer Qingrening Granule by microwave-assisted method were optimized as follows:the ethanol concentration was 70%;the microwave power was 255 W;the extracting time was 1 min and extracting temperature was 80℃.Under the optimized conditions,the recovery and the relative standard deviation of Baicalin were 96.9%～100.3%and 2.42%(n=6),respectively.Compared with ultrasound-assisted extraction and microwave-assisted extraction,MAE was simple and accurate with good reproducibility.
The results show that microwave-assisted extraction-RP-HPLC is a stable and reliable method for the determination of the content of Baicalin and Chlorogenic acid in TCMPP,and it can be used as a referrence for quality control of Chlorogenic acid and Baicalin in TCMPP.
黄芩苷和绿原酸存在于多种植物中,是许多中成药中药效成分。根据报道,黄芩苷和绿原酸均具有抗菌抗炎、消除自由基和抗氧化等作用。
本文针对银黄片和小儿清热宁颗粒中黄芩苷和绿原酸的微波辅助提取作了一系列的研究工作。
建立了采用微波辅助提取银黄片样品中绿原酸及黄芩苷、并以反相高效液相色谱法测定其含量的实验方法。分别通过单因素实验和正交实验设计,优化了萃取溶剂浓度、微波功率、微波辐射时间和微波提取温度四个提取条件,确定了微波辅助萃取法提取银黄片样品中的绿原酸及黄芩苷的最佳条件为:乙醇浓度70%,微波功率255W,提取时间1min,提取温度80℃。在上述最优条件下进行了精密度和回收率实验,绿原酸及黄芩苷加入回收率分别在96.2%～100.3%与96.5%～106.3%之间,RSD分别为3.69%(n=5)和4.03%(n=5)。
建立了采用微波辅助提取小儿清热宁颗粒样品中黄芩苷、并以反相高效液相色谱法测定其含量的实验方法。通过正交实验设计,优化了萃取溶剂浓度、微波功率、微波辐射时间和微波提取温度四个提取条件,确定了微波辅助萃取法提取小儿清热宁颗粒样品中的黄芩苷的最佳条件:提取溶剂为70%乙醇,微波功率为255W,微波提取时间为1min,提取温度为80℃。在上述最优条件下进行了精密度和回收率实验,黄芩苷加入回收率在96.9%～100.3%之间,RSD为2.42%(n=6)。与超声波提取法比较,微波辅助萃取法具有操作简便,快速,重现性好等特点。
通过以上两个体系的研究,可得出微波辅助提取-反相高效液相色谱法测定中成药中绿原酸及黄芩苷含量的方法稳定可靠,可为中成药中绿原酸及黄芩苷质量监控提供参考方法。
Traditional Chinese Medicine Patent Prescription(TCMPP) is a prescription which is produced in accordance with the provisions of the prescription,production processes and quality standards by Chinese herbal medicine under the guidence of Traditional Chinese Medicine(TCM) theory. TCMPP has many unique advantages,such as convenient to carry,easy to use, little toxicity and so on.With the modernization of TCM,TCMPP play more and more important role in the field of TCM.
Baicalin and Chlorogenic acid exist in many kinds of plants.They can be used as bioactive compounds in lots of TCMPP.It is reported that Baicalin and Chlorogenic acid have shown antibacterial,anti-inflammatory,significant scavenging of free oxygen radicals and antioxidative activity.
The microwave-assisted extraction of Baicalin and Chlorogenic acid of Yinhuang Tablets and Xiaoer Qingrening Granule was studied in this thesis.
Determination of Baicalin and Chlorogenic acid from Yinhuang Tablets by microwave-assisted extraction(MAE) and RP-HPLC was reported in the first part of thesis.The effects of solvent concentration,microwave power, extracting time and extracting temperature were evaluated by single factor and orthogonal experiments.The extraction conditions of Baicalin and Chlorogenic acid from Yinhuang Tablets by microwave-assisted method were optimized as follows:the ethanol concentration was 70%;the microwave power was 255 W;the extracting time was 1 min and extracting temperature was 80℃.Under the optimized conditions,the recovery of Baicalin and Chlorogenic acid were 96.2%～100.3%and 96.5%～106.3%,respectively.The relative standard deviation of Baicalin and Chlorogenic acid were 3.69%(n=5) and 4.03%(n=5),respectively.
Determination of Baicalin from Xiaoer Qingrening Granule by microwave-assisted extraction and RP-HPLC was reported in the second part of thesis.The effects of solvent concentration,microwave power,extracting time and extracting temperature were evaluated by orthogonal experiments. The extraction conditions of Baicalin from Xiaoer Qingrening Granule by microwave-assisted method were optimized as follows:the ethanol concentration was 70%;the microwave power was 255 W;the extracting time was 1 min and extracting temperature was 80℃.Under the optimized conditions,the recovery and the relative standard deviation of Baicalin were 96.9%～100.3%and 2.42%(n=6),respectively.Compared with ultrasound-assisted extraction and microwave-assisted extraction,MAE was simple and accurate with good reproducibility.
The results show that microwave-assisted extraction-RP-HPLC is a stable and reliable method for the determination of the content of Baicalin and Chlorogenic acid in TCMPP,and it can be used as a referrence for quality control of Chlorogenic acid and Baicalin in TCMPP.
引文
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