HPLC法测定新疆准噶尔乌头不同炮制品中单酯型生物碱的含量
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摘要
目的建立新疆准噶尔乌头中单酯型生物碱的高效液相色谱(high performance liquid chromatography,HPLC)含量测定方法。方法采用X Bridge C18色谱柱(250mm×4.6mm,5μm),以四氢呋喃-乙腈(3∶5)为流动相A,以0.1mol/L醋酸铵溶液(每1 000mL加冰醋酸0.5mL)为流动相B,进行梯度洗脱,检测波长为235nm。结果准噶尔乌头分别按药典法、高压蒸法、加辅料法炮制后双酯型生物碱水解为苯甲酰乌头碱,炮制方法不同,单酯型生物碱的含量也有所不同,准噶尔乌头中苯甲酰乌头原碱的含量约为制川乌的2/5,准噶尔乌头药典法炮制品中苯甲酰乌头原碱的含量与制川乌相似,准噶尔乌头高压蒸法炮制品中苯甲酰乌头原碱的含量约为制川乌的3.4倍,准噶尔乌头加辅料法炮制品中苯甲酰乌头原碱的含量约为制川乌的1/2,3种炮制品中单酯型生物碱含量大小依次为高压蒸法炮制品>药典法炮制品>加辅料法炮制品。结论准噶尔乌头炮制品中单酯型生物碱的HPLC含量测定方法简便、可行,为进一步开发和利用奠定了基础。
Objective To set up high performance liquid chromatography(HPLC) method of monoester alkaloids in Aconitum soongaricum and prepared products.Methods We used X Bridge C18 chromatographic column(250 mm×4.6 mm,5 μm),took tetrahydrofuran-acetonitrile(3∶5) as mobile phase A,0.1 mol/L Solution of ammonium acetate(each 1 000 mL added glacial acetic acid 0.5 mL) as mobile phase B,gradient elute,detected wavelength for 235 nm.Results Diester diterpenoid alkaloids in Aconitum soongaricum prepared were transformed to monoester alkaloids,the contents of its were different according to different prepareing methods.monoester alkaloids in Aconitum soongaricum was 2/5 of prepared radix aconite,monoester alkaloids in pharmacopeia prepared product of Aconitum soongaricum was similar to prepared radix aconite,monoester alkaloids in high-pressure steamed prepared product of Aconitum soongaricum was 3.4 times of prepared radix aconite,monoester alkaloids in adding accessories prepared product of Aconitum soongaricum was 1/2 of prepared radix aconite,the successive order of three prepared products were high-pressure steamed prepared product> pharmacopeia prepared product > adding accessories prepared product.Conclusion HPLC method is simple,accurate,high sensitivity,it can be used in determination of the monoester alkaloids from Aconitum soongaricum,which had potential medicinal value and are worthy of further being studied.
Objective To set up high performance liquid chromatography(HPLC) method of monoester alkaloids in Aconitum soongaricum and prepared products.Methods We used X Bridge C18 chromatographic column(250 mm×4.6 mm,5 μm),took tetrahydrofuran-acetonitrile(3∶5) as mobile phase A,0.1 mol/L Solution of ammonium acetate(each 1 000 mL added glacial acetic acid 0.5 mL) as mobile phase B,gradient elute,detected wavelength for 235 nm.Results Diester diterpenoid alkaloids in Aconitum soongaricum prepared were transformed to monoester alkaloids,the contents of its were different according to different prepareing methods.monoester alkaloids in Aconitum soongaricum was 2/5 of prepared radix aconite,monoester alkaloids in pharmacopeia prepared product of Aconitum soongaricum was similar to prepared radix aconite,monoester alkaloids in high-pressure steamed prepared product of Aconitum soongaricum was 3.4 times of prepared radix aconite,monoester alkaloids in adding accessories prepared product of Aconitum soongaricum was 1/2 of prepared radix aconite,the successive order of three prepared products were high-pressure steamed prepared product> pharmacopeia prepared product > adding accessories prepared product.Conclusion HPLC method is simple,accurate,high sensitivity,it can be used in determination of the monoester alkaloids from Aconitum soongaricum,which had potential medicinal value and are worthy of further being studied.
引文
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[5]国家药典委员会.中国药典(一部)[S].北京:化学工业出版社,2010:33-34.
[6]李飞,张世臣,杨蕾,等.浸泡时间及加热方式对川乌饮片质量的影响[J].北京中医药大学学报,1995,18(3):58-59.
[7]李飞,张世臣,杨蕾,等.正交设计法优选乌头炮制工艺[J].北京中医药大学学报,1998,21(1):38-39.
[8]张聿梅,鲁静,蒋渝.川乌和制川乌中单酯及双酯型生物碱成分的含量测定[J].药物分析杂志,2005,25(7):807-812.
[9]孙兰,周海燕,赵润怀.HPLC法同时测定附子中6种单酯和双酯型生物碱[J].中草药,2009,40(1):131-134.
[10]刘文龙,刘志强,宋凤瑞,等.乌头类双酯型生物碱组分转化为单酯水解型及脂型生物碱组分的研究[J].高等学校化学学报,2011,32(3):717-720.
[11]吴平丽,刘雯,卓超.应用高速逆流色谱技术从附子中分离制备苯甲酰新乌头原碱[J].中医药现代化,2009,11(2):260-262.
[12]黄志芳,易进海,陈东安.制川乌HPLC特征图谱研究和6种酯型生物碱的含量测定[J].药物分析杂志,2011,31(2):217-221.
[13]陈东安,易进海,黄志芳.附片指纹图谱研究及6种酯型生物碱含量测定[J].中国中药杂志,2010,35(21):2829-2833.
[14]吴超,赵翡翠,姜林.新疆准噶尔乌头及其炮制品的急性毒性和镇痛作用研究[J].新疆医科大学学报,2012,35(2):197-201.
[15]刘淑敏,聂继红,赵翡翠.分光光度法测定新疆乌头属植物总生物碱的含量[J].新疆医科大学学报,2012,35(2):193-196.
[2]新疆植物志编辑委员会.新疆植物志(第一卷,第二册)[M].乌鲁木齐:新疆科技卫生出版社,1999:231-242.
[3]张继,杨永利,王一峰,等.药用植物准噶尔乌头的研究[J].西北植物学报,1999,19(4):732-734.
[4]魏孝义,张继.准噶尔乌头二萜生物碱成分的研究[J].西北师范大学学报:自然科学版,1998,34(3):45-48.
[5]国家药典委员会.中国药典(一部)[S].北京:化学工业出版社,2010:33-34.
[6]李飞,张世臣,杨蕾,等.浸泡时间及加热方式对川乌饮片质量的影响[J].北京中医药大学学报,1995,18(3):58-59.
[7]李飞,张世臣,杨蕾,等.正交设计法优选乌头炮制工艺[J].北京中医药大学学报,1998,21(1):38-39.
[8]张聿梅,鲁静,蒋渝.川乌和制川乌中单酯及双酯型生物碱成分的含量测定[J].药物分析杂志,2005,25(7):807-812.
[9]孙兰,周海燕,赵润怀.HPLC法同时测定附子中6种单酯和双酯型生物碱[J].中草药,2009,40(1):131-134.
[10]刘文龙,刘志强,宋凤瑞,等.乌头类双酯型生物碱组分转化为单酯水解型及脂型生物碱组分的研究[J].高等学校化学学报,2011,32(3):717-720.
[11]吴平丽,刘雯,卓超.应用高速逆流色谱技术从附子中分离制备苯甲酰新乌头原碱[J].中医药现代化,2009,11(2):260-262.
[12]黄志芳,易进海,陈东安.制川乌HPLC特征图谱研究和6种酯型生物碱的含量测定[J].药物分析杂志,2011,31(2):217-221.
[13]陈东安,易进海,黄志芳.附片指纹图谱研究及6种酯型生物碱含量测定[J].中国中药杂志,2010,35(21):2829-2833.
[14]吴超,赵翡翠,姜林.新疆准噶尔乌头及其炮制品的急性毒性和镇痛作用研究[J].新疆医科大学学报,2012,35(2):197-201.
[15]刘淑敏,聂继红,赵翡翠.分光光度法测定新疆乌头属植物总生物碱的含量[J].新疆医科大学学报,2012,35(2):193-196.