高效液相色谱法同时测定蒙药复方述达格-4中6个成分的含量
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摘要
目的:建立采用HPLC同时测定蒙药复方述达格-4中1-苯基-7-(3-甲氧基-4-羟基)苯基-5-醇-3-庚酮、高良姜素、山柰素、高良姜素-3-甲醚、α-细辛醚、木香烃内酯含量的方法。方法:采用C18色谱柱(4.6 mm×250 mm,5μm),以乙腈-0.2%乙酸水溶液为流动相,梯度洗脱,流速0.6 mL·min~(-1),检测波长254 nm,柱温30℃,进样量为10μL。结果:1-苯基-7-(3-甲氧基-4-羟基)苯基-5-醇-3-庚酮、高良姜素、山柰素、高良姜素-3-甲醚、α-细辛醚、木香烃内酯的进样量与其峰面积具有良好的线性关系(r=0.999 9);平均加样回收率(n=6)为96.6%～101.1%,RSD为0.70%～1.8%;测定样品6批,1-苯基-7-(3-甲氧基-4-羟基)苯基-5-醇-3-庚酮、高良姜素、山柰素、高良姜素-3-甲醚、α-细辛醚、木香烃内酯的平均含量分别为0.008 4%～0.060 0%、0.010 7%～0.061 6%、0.010 9%～0.086 5%、0.006 2%～0.066 6%、0.011 0%～0.078 1%、0.005 1%～0.060 6%。结论:该方法可用于蒙药复方述达格-4的质量控制,可为蒙药复方述达格-4资源开发利用提供理论依据。
Objective:To establish a method for simultaneous determination of 6 components including 1-phenyl-7-(3-methoxy-4-hydroxy)phenyl-5-ol-3-heptanone,galangin,kaempferide,galangin-3-methylether,alpha-asarone and costunolide in Mongolian medicine compound formula Shudage-4 by HPLC. Methods:Separation was performed on a C18 column(4.6 mm×250 mm,5 μm)and the mobile phase consisted of acetonitrile-0.2% glacialacetic acid with gradient elution at a flow rate of 0.6 mL·min-1. The detection wavelength was 254 nm and the column temperature was 30 ℃. The injection volume was 10 μL. Results:1-phenyl-7-(3-methoxy-4-hydroxy)phenyl-5-ol-3-heptanone,galangin,kaempferide,galangin-3-methylether,alpha-asarone and costunolide exhibited good linear relationship with correlation coefficients of 0.999 9,the recoveries were 96.6%-101.1%,and the RSD were 0.70%-1.8%. The content ranges of the above mentioned components in 6 samples were 0.008 4%-0.060 0%,0.010 7%-0.061 6%,0.010 9%-0.086 5%,0.006 2%-0.066 6%,0.011 0%-0.078 1% and 0.005 1%-0.060 6%,respectively. Conclusion:The method can be applied in quality control of Mongolian medicine compound formula Shudage-4. The study can provide theoretical basis for development and utilization of Mongolian medicine Shudage-4.
Objective:To establish a method for simultaneous determination of 6 components including 1-phenyl-7-(3-methoxy-4-hydroxy)phenyl-5-ol-3-heptanone,galangin,kaempferide,galangin-3-methylether,alpha-asarone and costunolide in Mongolian medicine compound formula Shudage-4 by HPLC. Methods:Separation was performed on a C18 column(4.6 mm×250 mm,5 μm)and the mobile phase consisted of acetonitrile-0.2% glacialacetic acid with gradient elution at a flow rate of 0.6 mL·min-1. The detection wavelength was 254 nm and the column temperature was 30 ℃. The injection volume was 10 μL. Results:1-phenyl-7-(3-methoxy-4-hydroxy)phenyl-5-ol-3-heptanone,galangin,kaempferide,galangin-3-methylether,alpha-asarone and costunolide exhibited good linear relationship with correlation coefficients of 0.999 9,the recoveries were 96.6%-101.1%,and the RSD were 0.70%-1.8%. The content ranges of the above mentioned components in 6 samples were 0.008 4%-0.060 0%,0.010 7%-0.061 6%,0.010 9%-0.086 5%,0.006 2%-0.066 6%,0.011 0%-0.078 1% and 0.005 1%-0.060 6%,respectively. Conclusion:The method can be applied in quality control of Mongolian medicine compound formula Shudage-4. The study can provide theoretical basis for development and utilization of Mongolian medicine Shudage-4.
引文
[1]中华人民共和国卫生部药品标准蒙药分册[S].1998:158Drug Specifications Promulgated by the Ministry of Public Health,P.R.China.Mongolian Fascicles[S].1998:158
[2]贾鑫,董玉,武娜.紫外可见分光光度法测定蒙药述达格-4中总黄酮的含量[J].内蒙古医学院学报,2010,32(3):303JIA X,DONG Y,WU N.Determination of total flavones content in Shudage-4 by UV-visible spectrophotometry[J].J Inner Mongolia Med Coll,2010,32(3):303
[3]信莎莎,杜银飞,董玉.紫外可见分光光度法测定蒙药述达格-4中苯丙素的含量[J].内蒙古大学学报(自然科学版),2016,47(5):522XIN SS,DU YF,DONG Y.Determination of phenylpropanoids in Mongolian medicine compound formula Shudage-4 by UV-VISspectrophotometry[J].J Inner Mongolian Univ(Nat Sci Ed),2016,47(5):522
[4]信莎莎,杨洋,孙国园,等.HPLC法测定蒙药复方述达格-4中1-苯基-7-(3-甲氧基-4-羟基)苯基-5-醇-3-庚酮的含量[J].内蒙古大学学报(自然科学版),2015,46(2):191XIN SS,YANG Y,SUN GY,et al.Quantitative determination of1-phenyl-7-(3-methoxy-4-hydroxy)phenyl-5-ol-3-heptanone in Mongolian medicine compound formula Shudage-4 by HPLC[J].J Inner mongolian Univ(Nat Sci Ed),2015,46(2):191
[5]马强,贾鑫,董玉.RP-HPLC法测定蒙药复方述达格-4中高良姜素和山奈素的含量[J].北京中医药大学学报,2010,33(12):845MA Q,JIA X,DONG Y.Quantitative determination of galangin and kaempferide in Shudage-4(Mongolian medicinal formula)by RP-HPLC[J].J Beijing Univ Tradit Chin Med,2010,33(12):845
[6]信莎莎,杨洋,白埔,等.蒙药述达格-4抗小鼠胃溃疡的作用研究[J].北京中医药大学学报,2015,38(8):524XIN SS,YANG Y,BAI P,et al.Effects of Mongolian medicine Shudage-4 on gastric ulcer[J].J Beijing Univ Tradit Chin Med,2015,38(8):524
[7]杜银飞,周昊霏,信莎莎,等.蒙药复方述达格-4有效部位抗实验性胃溃疡的作用及其机制[J].北京中医药大学学报,2016,39(10):839DU YF,ZHOU HF,XIN SS,et al.Effect and mechanism of effective components of Mongolian medicine compound Shudage-4 against experimental stomach ulcer[J].J Beijing Univ Tradit Chin Med,2016,39(10):839
[8]祝永仙,李尚秀,赵升逵,等.高良姜的化学成分研究[J].云南民族大学学报(自然科学版),2013,22(4):239ZHU YX,LI SX,ZHAO SK,et al.Study on chemical constituents of Alpinia officinarum Hance[J].J Yunnan Univ Natl(Nat Sci Ed),2013,22(4):239
[9]董玉,石任兵,刘斌.石菖蒲化学成分的研究(Ⅰ)[J].北京中医药大学学报,2007,30(1):61DONG Y,SHI RB,LIU B.Study on chemical compositions of Acorus tatarinowii Schott(Ⅰ)[J].J Beijing Univ Tradit Chin Med,2007,30(1):61
[10]张婷,马林,吴丰,等.云木香乙醇提取物化学成分研究[J].中国中药杂志,2012,37(9):1232ZHANG T,MA L,WU F,et al.Study on chemical constituents of extracts of Radix Aucklandiae alcohol cloud[J].China J Chin Mater Med,2012,37(9):1232
[11]曹纬国,刘志勤,邵云,等.黄酮类化合物药理作用的研究进展[J].西北植物学报,2003,23(12):2241CAO WG,LIU ZQ,SHAO Y,et al.Research progress in pharmacological action of flavonoid[J].J Northwest Plant,2003,23(12):2241
[12]张丽娟,刘继勇,姚翀,等.洋川芎内酯类化合物药理作用研究进展[J].中国药学杂志,2015,50(13):1081ZHANG LJ,LIU JY,YAO C,et al.Progress of senkyunolide compounds pharmacological research[J].Chin Pharm J,2015,50(13):1081
[13]李洪福,李永辉,王勇,等.高良姜化学成分及药理活性的研究[J].中国实验方剂学杂志,2014,20(7):236LI HF,LI YH,WANG Y,et al.Advances in studies on chemical constituents in Alpiniae Officinarum Rhizoma and their pharmacological activities[J].Chin J Exp Tradit Med Form,2014,20(7):236
[14]赵李宏,吴建梅,武凤兰.α-细辛脑近10年研究概述[J].中国中药杂志,2007,32(7):562ZHAO LH,WU JM,WU FL.α-asarone takes nearly 10 years of research[J].China J Chin Mater Med,2007,32(7):562
[15]潘阳,王小静,潘娟,等.木香烃内酯的药理作用及构效关系研究进展[J].中南药学,2013,11(2):108PAN Y,WANG XJ,PAN J,et al.Research progress of pharmacological action and structure-activity relationship of costunolide[J].Cent Suoth Pharm,2013,11(2):108
[16]曹淑瑞,刘治勇,张雷,等.高效液相色谱法同时测定食品中6种对羟基苯甲酸酯[J].分析化学,2012,40(4):529CAO SR,LIU ZY,ZHANG L,et al.Simultaneous determination of 6 benzoic acid esters in food by high performance liquid chromatography[J].Anal Chem,2012,40(4):5292018 9 5
[2]贾鑫,董玉,武娜.紫外可见分光光度法测定蒙药述达格-4中总黄酮的含量[J].内蒙古医学院学报,2010,32(3):303JIA X,DONG Y,WU N.Determination of total flavones content in Shudage-4 by UV-visible spectrophotometry[J].J Inner Mongolia Med Coll,2010,32(3):303
[3]信莎莎,杜银飞,董玉.紫外可见分光光度法测定蒙药述达格-4中苯丙素的含量[J].内蒙古大学学报(自然科学版),2016,47(5):522XIN SS,DU YF,DONG Y.Determination of phenylpropanoids in Mongolian medicine compound formula Shudage-4 by UV-VISspectrophotometry[J].J Inner Mongolian Univ(Nat Sci Ed),2016,47(5):522
[4]信莎莎,杨洋,孙国园,等.HPLC法测定蒙药复方述达格-4中1-苯基-7-(3-甲氧基-4-羟基)苯基-5-醇-3-庚酮的含量[J].内蒙古大学学报(自然科学版),2015,46(2):191XIN SS,YANG Y,SUN GY,et al.Quantitative determination of1-phenyl-7-(3-methoxy-4-hydroxy)phenyl-5-ol-3-heptanone in Mongolian medicine compound formula Shudage-4 by HPLC[J].J Inner mongolian Univ(Nat Sci Ed),2015,46(2):191
[5]马强,贾鑫,董玉.RP-HPLC法测定蒙药复方述达格-4中高良姜素和山奈素的含量[J].北京中医药大学学报,2010,33(12):845MA Q,JIA X,DONG Y.Quantitative determination of galangin and kaempferide in Shudage-4(Mongolian medicinal formula)by RP-HPLC[J].J Beijing Univ Tradit Chin Med,2010,33(12):845
[6]信莎莎,杨洋,白埔,等.蒙药述达格-4抗小鼠胃溃疡的作用研究[J].北京中医药大学学报,2015,38(8):524XIN SS,YANG Y,BAI P,et al.Effects of Mongolian medicine Shudage-4 on gastric ulcer[J].J Beijing Univ Tradit Chin Med,2015,38(8):524
[7]杜银飞,周昊霏,信莎莎,等.蒙药复方述达格-4有效部位抗实验性胃溃疡的作用及其机制[J].北京中医药大学学报,2016,39(10):839DU YF,ZHOU HF,XIN SS,et al.Effect and mechanism of effective components of Mongolian medicine compound Shudage-4 against experimental stomach ulcer[J].J Beijing Univ Tradit Chin Med,2016,39(10):839
[8]祝永仙,李尚秀,赵升逵,等.高良姜的化学成分研究[J].云南民族大学学报(自然科学版),2013,22(4):239ZHU YX,LI SX,ZHAO SK,et al.Study on chemical constituents of Alpinia officinarum Hance[J].J Yunnan Univ Natl(Nat Sci Ed),2013,22(4):239
[9]董玉,石任兵,刘斌.石菖蒲化学成分的研究(Ⅰ)[J].北京中医药大学学报,2007,30(1):61DONG Y,SHI RB,LIU B.Study on chemical compositions of Acorus tatarinowii Schott(Ⅰ)[J].J Beijing Univ Tradit Chin Med,2007,30(1):61
[10]张婷,马林,吴丰,等.云木香乙醇提取物化学成分研究[J].中国中药杂志,2012,37(9):1232ZHANG T,MA L,WU F,et al.Study on chemical constituents of extracts of Radix Aucklandiae alcohol cloud[J].China J Chin Mater Med,2012,37(9):1232
[11]曹纬国,刘志勤,邵云,等.黄酮类化合物药理作用的研究进展[J].西北植物学报,2003,23(12):2241CAO WG,LIU ZQ,SHAO Y,et al.Research progress in pharmacological action of flavonoid[J].J Northwest Plant,2003,23(12):2241
[12]张丽娟,刘继勇,姚翀,等.洋川芎内酯类化合物药理作用研究进展[J].中国药学杂志,2015,50(13):1081ZHANG LJ,LIU JY,YAO C,et al.Progress of senkyunolide compounds pharmacological research[J].Chin Pharm J,2015,50(13):1081
[13]李洪福,李永辉,王勇,等.高良姜化学成分及药理活性的研究[J].中国实验方剂学杂志,2014,20(7):236LI HF,LI YH,WANG Y,et al.Advances in studies on chemical constituents in Alpiniae Officinarum Rhizoma and their pharmacological activities[J].Chin J Exp Tradit Med Form,2014,20(7):236
[14]赵李宏,吴建梅,武凤兰.α-细辛脑近10年研究概述[J].中国中药杂志,2007,32(7):562ZHAO LH,WU JM,WU FL.α-asarone takes nearly 10 years of research[J].China J Chin Mater Med,2007,32(7):562
[15]潘阳,王小静,潘娟,等.木香烃内酯的药理作用及构效关系研究进展[J].中南药学,2013,11(2):108PAN Y,WANG XJ,PAN J,et al.Research progress of pharmacological action and structure-activity relationship of costunolide[J].Cent Suoth Pharm,2013,11(2):108
[16]曹淑瑞,刘治勇,张雷,等.高效液相色谱法同时测定食品中6种对羟基苯甲酸酯[J].分析化学,2012,40(4):529CAO SR,LIU ZY,ZHANG L,et al.Simultaneous determination of 6 benzoic acid esters in food by high performance liquid chromatography[J].Anal Chem,2012,40(4):5292018 9 5