HPLC法同时测定蒙药复方述达格-4血清中6种成分的含量
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摘要
目的建立HPLC同时测定蒙药复方述达格-4血清中1-苯基-7-(3-甲氧基-4-羟基)苯基-5-醇-3-庚酮、高良姜素、山奈素、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Agilent C18色谱柱(4.6 mm×250 mm,5μm),乙腈(A)-0.2%乙酸水溶液(B)为流动相,流速0.6m L/min,柱温30℃,进样量为100μL,检测波长254 nm。结果 1-苯基-7-(3-甲氧基-4-羟基)苯基-5-醇-3-庚酮、高良姜素、山奈素、高良姜素-3-甲醚、α-细辛醚、木香烃内酯的质量浓度与其峰面积具有良好的线性关系(r=0.999 0~0.999 8)。平均加样回收率(n=6)分别为91.74%~102.10%,RSD为1.03%~2.61%;1-苯基-7-(3-甲氧基-4-羟基)苯基-5-醇-3-庚酮、高良姜素、山奈素、高良姜素-3-甲醚、α-细辛醚、木香烃内酯的平均含量分别为3.200 0、0.647 5、0.865 6、0.156 0、0.331 9、3.075 1 mg/L。结论该方法操作简便、稳定、重复性好,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血清药物化学研究奠定基础。
Objective To establish a method for simultaneously determining the content of 1-phenyl-7-(3-methoxy-4-hydroxy) phenyl-5-ol-3-heptanone,galangin,kaempferide,galangin-3-methylether,α-asarone and costunolide in serum from Mongolian medicine compound formula-Shudage-4 by using HPLC.Methods The HPLC procedure was performed on the chromatographic column of Agilent C18(4. 6 mm ×250 mm,5 μm) at 30℃,and mobile phase was acetonitrile(A)-0. 2% water solution of acetic acid(B) in gradient elution. The flow velocity was 0. 6 m L/min,sample size was 100 μL and detection wavelength was 254 nm. Results The mass concentration and peak areas of 1-phenyl-7-(3-methoxy-4-hydroxy) phenyl-5-ol-3-heptanone, galangin, kaempferide, galangin-3-methylether, α-asarone and costunolide showed good linear relationships(r = 0. 999 0-0. 999 8). The average recoveries of samples(n = 6) were 91. 74%-102. 10%,and RSD were 1. 03%-2. 61%. The average content of 1-phenyl-7-(3-methoxy-4-hydroxy) phenyl-5-ol-3-heptanone,galangin,kaempferide,galangin-3-methylether,α-asarone and costunolide was,respectively,3. 200 0 mg/L,0. 647 5 mg/L,0. 865 6 mg/L,0. 156 0 mg/L,0. 331 9 mg/L and 3. 075 1 mg/L. Conclusion The method is easy and stable with higher repeatability,and it can be used in quality control of Shudage-4 and provide a basis for serum pharmacochemistry study of Shudage-4 resources.
Objective To establish a method for simultaneously determining the content of 1-phenyl-7-(3-methoxy-4-hydroxy) phenyl-5-ol-3-heptanone,galangin,kaempferide,galangin-3-methylether,α-asarone and costunolide in serum from Mongolian medicine compound formula-Shudage-4 by using HPLC.Methods The HPLC procedure was performed on the chromatographic column of Agilent C18(4. 6 mm ×250 mm,5 μm) at 30℃,and mobile phase was acetonitrile(A)-0. 2% water solution of acetic acid(B) in gradient elution. The flow velocity was 0. 6 m L/min,sample size was 100 μL and detection wavelength was 254 nm. Results The mass concentration and peak areas of 1-phenyl-7-(3-methoxy-4-hydroxy) phenyl-5-ol-3-heptanone, galangin, kaempferide, galangin-3-methylether, α-asarone and costunolide showed good linear relationships(r = 0. 999 0-0. 999 8). The average recoveries of samples(n = 6) were 91. 74%-102. 10%,and RSD were 1. 03%-2. 61%. The average content of 1-phenyl-7-(3-methoxy-4-hydroxy) phenyl-5-ol-3-heptanone,galangin,kaempferide,galangin-3-methylether,α-asarone and costunolide was,respectively,3. 200 0 mg/L,0. 647 5 mg/L,0. 865 6 mg/L,0. 156 0 mg/L,0. 331 9 mg/L and 3. 075 1 mg/L. Conclusion The method is easy and stable with higher repeatability,and it can be used in quality control of Shudage-4 and provide a basis for serum pharmacochemistry study of Shudage-4 resources.
引文
[1]王喜军.中药及中药复方的血清药物化学研究[J].世界科学技术—中医药现代化,2002,4(2):1-5.Wang XJ.Studies on serum pharmacochemistry of traditional Chinese medicine[J].World Science and Technology/Modernization of Traditional Chinese Medicine and Materia Medica,2002,4(2):1-5.
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[5]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):303-305.Jia X,Dong Y,Wu N.Determination of total flavones content in Shudage-4 by UV-visible spectrophotometry[J].Journal of Inner Mongolia Medical College,2010,32(3):303-305.
[6]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):845-847.Ma Q,Jia X,Dong Y.Quantitative determination of galangin and kaempferide in Shudage-4(Mongolian medicinal formula)by RP-HPLC[J].Journal of Beijing University of Traditional Chinese Medicine,2010,33(12):845-847.
[7]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):524-528.Xin SS,Yang Y,Bai P,et al.Effects of Mongolian formula Shudage-4 on gastric ulcer[J].Journal of Beijing University of Traditional Chinese Medicine,2015,38(8):524-528.
[8]杜银飞,周昊菲,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):839-843.Du YF,Zhou HF,Xin SS.Effect and mechanism of effective components of Mongolian medicine compound Shudage-4 against experimental stomach ulcer[J].Journal of Beijing University of Traditional Chinese Medicine,2016,39(10):839-843.
[9]王喜军.中药血清药物化学的研究动态及发展趋势[J].中国中药杂志,2006,31(10):789-792.Wang XJ.Progress and future developing of the serum pharmacochemistry of traditional Chinese medicine[J].China Journal of Chinese Materia Medica,2006,31(10):789-792
[2]国家药典委员会.中华人民共和国卫生部药品标准:蒙药分册[M].呼和浩特:内蒙古科学技术出版社,1998:163.National Pharmacopoeia Commission of China.Fascicule of Mongolian Medicine,Drug Standard of Ministry of Health of the People’s Republic of China[M].Hohhot:Inner Mongolia Science and Technology Press,1998:163.
[3]杨洋,贾鑫,董玉,等.蒙药述达格-4的化学成分研究[J].内蒙古大学学报(自然科学版),2013,44(4):392-396.Yang Y,Jia X,Dong Y,et al.A study on the chemical components of the Mongolian medicine Shudage-4[J].Journal of Inner Mongolia University(Natural Science Edition),2013,44(4):392-396.
[4]信莎莎,杜银飞,贾鑫,等.蒙药复方述达格-4化学成分的分离与结构鉴定[J].北京中医药大学学报,2016,39(11):941-944.Xin SS,Du YF,Jia X,et al.Separation and identification of chemical constituents of Mongolian medicine compound Shudage-4[J].Journal of Beijing University of Traditional Chinese Medicine,2016,39(11):941-944.
[5]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):303-305.Jia X,Dong Y,Wu N.Determination of total flavones content in Shudage-4 by UV-visible spectrophotometry[J].Journal of Inner Mongolia Medical College,2010,32(3):303-305.
[6]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):845-847.Ma Q,Jia X,Dong Y.Quantitative determination of galangin and kaempferide in Shudage-4(Mongolian medicinal formula)by RP-HPLC[J].Journal of Beijing University of Traditional Chinese Medicine,2010,33(12):845-847.
[7]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):524-528.Xin SS,Yang Y,Bai P,et al.Effects of Mongolian formula Shudage-4 on gastric ulcer[J].Journal of Beijing University of Traditional Chinese Medicine,2015,38(8):524-528.
[8]杜银飞,周昊菲,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):839-843.Du YF,Zhou HF,Xin SS.Effect and mechanism of effective components of Mongolian medicine compound Shudage-4 against experimental stomach ulcer[J].Journal of Beijing University of Traditional Chinese Medicine,2016,39(10):839-843.
[9]王喜军.中药血清药物化学的研究动态及发展趋势[J].中国中药杂志,2006,31(10):789-792.Wang XJ.Progress and future developing of the serum pharmacochemistry of traditional Chinese medicine[J].China Journal of Chinese Materia Medica,2006,31(10):789-792