胆南星发酵制品与混合蒸制品的鉴别研究
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摘要
目的:以猪胆汁及天南星、制天南星为原料分别制备发酵制胆南星及混合蒸制胆南星,以胆汁酸类成分为指标,建立以猪胆汁为炮制辅料的胆南星2种炮制品的薄层鉴别及HPLC-ELSD特征图谱。方法:采用硅胶G薄层板,以石油醚:丙酮:冰醋酸(11∶8∶0. 8)为展开剂,10%硫酸乙醇溶液为显色剂,建立薄层色谱鉴别方法。采用Agilent Eclipse XDB C_(18)(4. 6 mm×250 mm,5μm)色谱柱,以乙腈与0. 1%冰醋酸水为流动相进行梯度洗脱,流速为1 m L/min,柱温为30℃,ELSD:漂移管温度为105℃,氮气流量为2. 5 m L/min,建立胆南星HPLC-ELSD特征图谱鉴别方法。结果:TLC和HPLC-ELSD图谱均显示发酵制胆南星可检测到游离型胆汁酸类成分猪胆酸(HCA)、猪去氧胆酸(HDCA)和鹅去氧胆酸(CDCA)3个特征成分,而混合蒸制胆南星中未检测出;混合蒸制胆南星可检测到结合型胆汁酸类成分甘氨猪去氧胆酸(GHDCA)和甘氨鹅去氧胆酸(GCDCA) 2个特征成分,而发酵制胆南星中未检测出。结论:所建胆汁酸类成分的薄层色谱鉴别法(TLC)和高效液相色谱-蒸发光散射法(HPLC-ELSD)均可有效鉴别胆南星的发酵制品和混合蒸制品,为胆南星质量控制提供依据。
Objective: Using pig bile and Arisaematis Rhizome and Arisaematis Rhizoma Preparatum as raw materials,the fermenting and mixed evaporating of arisaema cum bile were prepared respectively,and the bile acids were used as the index. To establish thin layer identification and HPLC-ELSD characteristic map of 2 processed products from porcine bile. Methods Silica gel G thin layer plate was applied,and petroleum ether: acetone: glacial acetic acid( 11∶ 8∶ 0. 8) were used as developing agent and 10% sulfuric acid ethanol solution as chromogenic agent,a TLC identification method was established. An Agilent Eclipse XDB C_(18)( 4. 6 mm × 250 mm,5 μm) column was used,with acetonitrile and 0. 1% glacial acetic acid water as mobile phase for gradient elution.The flow rate was 1 mL/min,at 30 ℃ and ELSD: drift tube at 105 ℃. The identification method of HPLC-ELSD characteristic map of arisaema cum bile was established by nitrogen flow rate of 2. 5 mL/min. Results: TLC and HPLC-ELSD spectra showed that three characteristic components of free hyocholic acid( HCA),hyodeoxycholic acid( HDCA) and chenodeoxycholic acid( CDCA),could be detected in fermented arisaema cum bile,but not in mixed evaporation. Two characteristic components of conjugated bile acids,( GHDCA) and( GCDCA),could be detected by mixed evaporation of arisaema cum bile,but not in the fermentation of arisaema cum bile. Conclusion: TLC and HPLC-ELSD can be used to identify the fermented and mixed distilled products of arisaema cum bile which can provide the basis for the quality control of arisaema cum bile.
Objective: Using pig bile and Arisaematis Rhizome and Arisaematis Rhizoma Preparatum as raw materials,the fermenting and mixed evaporating of arisaema cum bile were prepared respectively,and the bile acids were used as the index. To establish thin layer identification and HPLC-ELSD characteristic map of 2 processed products from porcine bile. Methods Silica gel G thin layer plate was applied,and petroleum ether: acetone: glacial acetic acid( 11∶ 8∶ 0. 8) were used as developing agent and 10% sulfuric acid ethanol solution as chromogenic agent,a TLC identification method was established. An Agilent Eclipse XDB C_(18)( 4. 6 mm × 250 mm,5 μm) column was used,with acetonitrile and 0. 1% glacial acetic acid water as mobile phase for gradient elution.The flow rate was 1 mL/min,at 30 ℃ and ELSD: drift tube at 105 ℃. The identification method of HPLC-ELSD characteristic map of arisaema cum bile was established by nitrogen flow rate of 2. 5 mL/min. Results: TLC and HPLC-ELSD spectra showed that three characteristic components of free hyocholic acid( HCA),hyodeoxycholic acid( HDCA) and chenodeoxycholic acid( CDCA),could be detected in fermented arisaema cum bile,but not in mixed evaporation. Two characteristic components of conjugated bile acids,( GHDCA) and( GCDCA),could be detected by mixed evaporation of arisaema cum bile,but not in the fermentation of arisaema cum bile. Conclusion: TLC and HPLC-ELSD can be used to identify the fermented and mixed distilled products of arisaema cum bile which can provide the basis for the quality control of arisaema cum bile.
引文
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[14]鄢海燕,邹纯才.四种动物胆粉中胆酸类成分分析及药理作用比较[J].皖南医学院学报,2012,31(4):274-277.
[15]赵启苗,单国顺,陈江宁,等.胆南星质量评价方法初探[J].中国实验方剂学杂志,2017,23(6):28-31.
[16]黎量,李欣逸,艾莉.胆南星炮制及质量标准研究进展与思考[J].中药与临床,2015,6(3):7-9.
[17]姚志昂,郭力,周娟,等.三十一批胆南星的对比研究[J].成都中医药大学学报,2011,34(3):57-59.
[18]贲永光,李康,李坤平,等.胆南星的薄层色谱鉴别[J].广东药学院学报,2009,25(2):160-161.
[2]李瑶.胆南星炮制前后成分变化及质量标准研究[D].南京:南京中医药大学,2018.
[3]陈云,郁红礼,吴皓,等.发酵对胆南星中胆汁酸类成分的影响及胆南星中3种游离胆汁酸含量测定研究[J].中国中药杂志,2018,43(22):4457-4461.
[4]吴仪洛.本草从新[M].上海:上海科学技术出版社,1958:100.
[5]太平惠民和剂局.太平惠民和剂局方[M].北京:人民卫生出版社,1985:18.
[6]曾世荣.活幼心书[M].北京:中国书店,1985:46.
[7]成都中医学院.中药炮制学[M].上海:上海科学技术出版社,1980:142.
[8]刘养清,刘二保.动物胆汁理化特性及药用[M].北京:化学工业出版社,2002:74-92.
[9]石岩,耿颖,郑天骄,等.猪胆粉HPLC-ELSD全轮廓谱图主要胆汁酸测定及化学计量学分析[J].药物分析杂志,2017,37(2):283.
[10]杨伟鹏,王怡薇,王彦礼,等.不同胆汁炮制方法对天南星解毒存效作用的实验研究[J].中国实验方剂学杂志,2009,15(12):33-35.
[11]赫炎,王孝涛.胆南星不同炮制品的药效和毒性实验研究[J].中药材,1997,20(9):459-461.
[12]游元元,万德光.动物胆汁药用研究进展[J].贵阳中医学院学报,2007,29(4):58-61.
[13]石岩,耿颖,郑天骄,等.猪胆粉HPLC-ELSD全轮廓谱图主要胆汁酸测定及化学计量学分析[J].药物分析杂志,2017,37(2):283.
[14]鄢海燕,邹纯才.四种动物胆粉中胆酸类成分分析及药理作用比较[J].皖南医学院学报,2012,31(4):274-277.
[15]赵启苗,单国顺,陈江宁,等.胆南星质量评价方法初探[J].中国实验方剂学杂志,2017,23(6):28-31.
[16]黎量,李欣逸,艾莉.胆南星炮制及质量标准研究进展与思考[J].中药与临床,2015,6(3):7-9.
[17]姚志昂,郭力,周娟,等.三十一批胆南星的对比研究[J].成都中医药大学学报,2011,34(3):57-59.
[18]贲永光,李康,李坤平,等.胆南星的薄层色谱鉴别[J].广东药学院学报,2009,25(2):160-161.