HPLC法测定中药常山散中常山乙素、常山甲素的系统适用性研究
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摘要
【目的】为制订中药常山散的国家质量标准和指导临床科学用药,进行了高效液相色谱法测定常山乙素、常山甲素含量的系统适用性研究.【方法】选择3种不同类型的液相和色谱柱,包括安捷伦1290型液相色谱仪(配套SB-C_(18)色谱柱)、沃特斯2695型液相色谱仪(配套XTerra@MS C_(18)色谱柱)和岛津SPD-10A型液相色谱仪(配套Amethyst C_(18)-H色谱柱).流动相:乙腈-0.3%冰醋酸(30∶70),三乙胺调pH值至5.2～6.2,流速:1.0mL/min,检测波长:265nm,柱温:25℃,进样量:10μL.【结果】3种类型的高效液相检测结果表明,三批次常山散中常山乙素和常山甲素的含量基本一致,常山乙素和常山甲素峰型较好,与周围杂质分离度较好.【结论】以上色谱条件可用来检测常山散中常山乙素和常山甲素的含量,适用于中药常山散及其相关制剂的质量控制,具有操作简便、稳定性好、精密度高等优点.
【Objective】In order to establish the national quality standard of Dichroa febrifugapowder and guide the clinical medication,the system suitability of high performance liquid chromatography(HPLC)method was studied for the test ofβ-dichroine andα-dichroine in D.febrifugapowder.【Method】Three different types of liquid phase and chromatographic column were chosen,including Agilent 1290 type liquid chromatograph(supporting SB-C_(18) chromatographic column),Waters 2695 type liquid chromatograph(supporting XTerra@ MS C_(18) chromatographic column)and Island ferry SPD-10 Atype liquid chromatograph(supporting the Amethyst C_(18)-H chromatographic column).Mobile phase:acetonitrile-0.3%glacial acetic acid(30∶70)and pH value to 5.2～6.2 adjusted with triethylamine,1.0 mL/min of velocity,265 nm of detection wavelength,25 ℃ of column temperature and 10μL of sample volume.【Result】The contents ofβ-dichroine andα-dichroine in 3 batches of D.febrifugapowder from 3 HPLC methods were similar,and better peak type and better separation effect were obtained.【Conclusion】The tested chromatography conditions could be used to detect contents ofβ-dichroine andα-dichroine for the quality control of D.febrifugapowder because of the easy operation,better stability and precision.
【Objective】In order to establish the national quality standard of Dichroa febrifugapowder and guide the clinical medication,the system suitability of high performance liquid chromatography(HPLC)method was studied for the test ofβ-dichroine andα-dichroine in D.febrifugapowder.【Method】Three different types of liquid phase and chromatographic column were chosen,including Agilent 1290 type liquid chromatograph(supporting SB-C_(18) chromatographic column),Waters 2695 type liquid chromatograph(supporting XTerra@ MS C_(18) chromatographic column)and Island ferry SPD-10 Atype liquid chromatograph(supporting the Amethyst C_(18)-H chromatographic column).Mobile phase:acetonitrile-0.3%glacial acetic acid(30∶70)and pH value to 5.2～6.2 adjusted with triethylamine,1.0 mL/min of velocity,265 nm of detection wavelength,25 ℃ of column temperature and 10μL of sample volume.【Result】The contents ofβ-dichroine andα-dichroine in 3 batches of D.febrifugapowder from 3 HPLC methods were similar,and better peak type and better separation effect were obtained.【Conclusion】The tested chromatography conditions could be used to detect contents ofβ-dichroine andα-dichroine for the quality control of D.febrifugapowder because of the easy operation,better stability and precision.
引文
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[7]谢秀满,孙万阳,黄竞怡,等.基于高压制备液相的多维色谱技术在中药分离纯化中的应用[J].分析化学,2016,44(7):1140-1147.
[8]孙艳妮,张宁,王翠玲,等.高效液相色谱法鉴别及测定中药吴茱萸中的生物胺[J].分析化学,2014,42(2):273-277.
[9]郑金聪,林王椿,姚步华.高效液相色谱法测定丹参酮ⅡA含量的系统适用性研究[J].中国医药导报,2010,7(32):49-50.
[10]杨家爱,曹天海.各国药典液相色谱方法系统适用性试验的比较[J].中国药事,2013,27(12):1305-1307.
[11]国家药典委员会.中华人民共和国药典[M].北京:中国医药科技出版社,2015:313.
[2]郭志廷,刘晓璐,梁剑平,等.常山碱及其衍生物药理活性研究进展[J].中兽医医药杂志,2014(2):17-18.
[3]ZHU S R,CHANDRASHEKAR G,MENG L,et al.Febrifugine analogue compounds:Synthesis and antimalarial evaluation[J].Bioorg Med Chem,2012,20(2):927-932.
[4]KIRANDEEP K,MEENAKSHI J,TARANDEEP K,et al.Antimalarials from nature[J].Bioorg Med Chem,2009,17(9):3229-3256.
[5]MURATA K,TAKANO F,FUSHIYA S,et al.Enhancement of NO production in activated macrophages in vivo by an antimalarial crude drug,Dichroa febrifuga[J].J Nat Prod,1998,61(6):729-733.
[6]李燕,刘明川,金林红,等.常山化学成分及生物活性研究进展[J].广州化工,2011,39(9):7-9.
[7]谢秀满,孙万阳,黄竞怡,等.基于高压制备液相的多维色谱技术在中药分离纯化中的应用[J].分析化学,2016,44(7):1140-1147.
[8]孙艳妮,张宁,王翠玲,等.高效液相色谱法鉴别及测定中药吴茱萸中的生物胺[J].分析化学,2014,42(2):273-277.
[9]郑金聪,林王椿,姚步华.高效液相色谱法测定丹参酮ⅡA含量的系统适用性研究[J].中国医药导报,2010,7(32):49-50.
[10]杨家爱,曹天海.各国药典液相色谱方法系统适用性试验的比较[J].中国药事,2013,27(12):1305-1307.
[11]国家药典委员会.中华人民共和国药典[M].北京:中国医药科技出版社,2015:313.