LC-MS/MS法同时测定复方丹参颗粒和复方丹参滴丸中6种成分
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摘要
目的建立LC-MS/MS法同时测定复方丹参颗粒和复方丹参滴丸(丹参、三七、冰片)中丹参素钠、三七皂苷R1、人参皂苷Re、人参皂苷Rg1、人参皂苷Rb1、丹参酮ⅡA的含有量。方法 2种药物75%甲醇提取液的分析采用Eclipse Plus C18色谱柱(3. 0 mm×150 mm,3. 5μm);流动相乙腈-0. 1%甲酸,梯度洗脱;体积流量0. 3 m L/min。结果 6种成分在各自范围内线性关系良好(R2≥0. 995 9),平均加样回收率95. 76%～105. 74%,RSD 1. 86%～4. 88%。除丹参素钠外,其他5种成分在复方丹参颗粒中的含有量均高于在复方丹参滴丸中。结论复方丹参颗粒和复方丹参滴丸中主要成分含有量有明显差异,可能会影响临床疗效。
AIM To establish an LC-MS/MS method for the simultaneous content determination of sodium danshensu,notoginsenoside R1,ginsenoside Re,ginsenoside Rg1,ginsenoside Rb1 and tanshinone ⅡAin Compound Danshen Granules and Compound Danshen Dropping Pills( Salviae miltiorrhizae Radix et Rhizoma,Notoginseng Radix et Rhizoma,Borneolum Syntheticum). METHODS The analysis of 75% methanol extracts of these two drugs were performed on an Eclipse Plus C18column( 3. 0 mm × 150 mm,3. 5 μm),with the mobile phase comprising of acetonitrile-0. 1%formic acid flowing at 0. 3 m L/min in a gradient elution manner. RESULTS Six constituents showed good linear relationships within their own ranges( R2≥0. 995 9),whose average recoveries were 95. 76%-105. 74% with the RSDs of 1. 86%-4. 88%. Except for sodium danshensu,the other five constituents in Compound Danshen Granules demonstrated higher contents than those in Compound Danshen Dropping Pills.CONCLUSION The obvious content difference of main components in Compound Danshen Granules and Compound Danshen Dropping Pills may affect clinical efficacy.
AIM To establish an LC-MS/MS method for the simultaneous content determination of sodium danshensu,notoginsenoside R1,ginsenoside Re,ginsenoside Rg1,ginsenoside Rb1 and tanshinone ⅡAin Compound Danshen Granules and Compound Danshen Dropping Pills( Salviae miltiorrhizae Radix et Rhizoma,Notoginseng Radix et Rhizoma,Borneolum Syntheticum). METHODS The analysis of 75% methanol extracts of these two drugs were performed on an Eclipse Plus C18column( 3. 0 mm × 150 mm,3. 5 μm),with the mobile phase comprising of acetonitrile-0. 1%formic acid flowing at 0. 3 m L/min in a gradient elution manner. RESULTS Six constituents showed good linear relationships within their own ranges( R2≥0. 995 9),whose average recoveries were 95. 76%-105. 74% with the RSDs of 1. 86%-4. 88%. Except for sodium danshensu,the other five constituents in Compound Danshen Granules demonstrated higher contents than those in Compound Danshen Dropping Pills.CONCLUSION The obvious content difference of main components in Compound Danshen Granules and Compound Danshen Dropping Pills may affect clinical efficacy.
引文
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[12]赵欣,强光辉,郭毅,等.复方丹参滴丸人含药血浆中三七相关代谢物的研究[J].质谱学报,2007,28(1):23-26,30.
[13] Pei W J,Zhao X F,Zhu Z M,et al. Study of the determination and pharmacokinetics of Compound Danshen Dripping Pills in human serum by column switching liquid chromatography electrospray ion trap mass spectrometry[J]. J Chromatogr B Analyt Technol Biomed Life Sci,2004,809(2):237-242.
[14]裴渭静,赵新锋,胡震,等.采用柱切换色谱离子阱质谱联用法研究复方丹参滴丸中丹参素及其代谢产物[J].分析化学,2005,33(4):505-508.
[2] Zhou L M,Zuo Z,Chow M S S. Danshen:an overview of its chemistry,pharmacology, pharmacokinetics and clinical use[J]. J Clin Pharmacol,2005,45(12):1345-1359.
[3]赵永娇,荆鲁.复方丹参制剂的优化研究概况[J].中国中药杂志,2011,36(17):2437-2440.
[4] Su C Y,Ming Q L,Rahman K,et al. Salvia miltiorrhiza:Traditional medicinal uses,chemistry,and pharmacology[J]. Chin J Nat Med,2015,13(3):163-182.
[5]马珂,汤金土.三七皂苷的实验研究进展[J].浙江中西医结合杂志,2002,12(3):197-199.
[6]商洪才,高秀梅,张伯礼,等.复方丹参方标本同治机制的诠释[J].中国中医基础医学杂志,2003,9(9):43-44.
[7] Zhu D,Wu L,Li C R,et al. Ginsenoside Rg1 protects rat cardiomyocyte from hypoxia/reoxygenation oxidative injury via antioxidant and intracellular calcium homeostasis[J]. J Cell Biochem,2009,108(1):117-124.
[8]国家药典委员会.中华人民共和国药典:2015年版一部[S].北京:中国医药科技出版社,2015:1213-1219.
[9]束云,李贻奎,李连达.复方丹参制剂药理作用的比较研究[J].中药药理与临床,2012,28(1):132-134.
[10]李玉珍,陈日来,陈晓凯,等.高效液相色谱法测定复方丹参片和滴丸中丹酚酸B和丹参酮ⅡA的含量[J].中国医院药学杂志,2005,25(6):523-525.
[11]邢俊波,方白玉.复方丹参制剂中活性成分的HPLC同时定量分析[J].中国中药杂志,2003,28(1):36-38.
[12]赵欣,强光辉,郭毅,等.复方丹参滴丸人含药血浆中三七相关代谢物的研究[J].质谱学报,2007,28(1):23-26,30.
[13] Pei W J,Zhao X F,Zhu Z M,et al. Study of the determination and pharmacokinetics of Compound Danshen Dripping Pills in human serum by column switching liquid chromatography electrospray ion trap mass spectrometry[J]. J Chromatogr B Analyt Technol Biomed Life Sci,2004,809(2):237-242.
[14]裴渭静,赵新锋,胡震,等.采用柱切换色谱离子阱质谱联用法研究复方丹参滴丸中丹参素及其代谢产物[J].分析化学,2005,33(4):505-508.