HPLC-DAD-ESI-MSn分析双黄连注射液中22个化学成分
Analysis of chemical constituents of Shuanghuanglian injection by HPLC-DAD-ESI-MSn
分类号:R917
出版年·卷·期(页码):2020,40 (2):321-328
DOI:
10.16155/j.0254-1793.2017.01.01
-----摘要:-------------------------------------------------------------------------------------------
目的: 采用高效液相色谱(HPLC)-DAD-ESI-MSn联用技术分析双黄连注射液中化学成分。方法: 采用Phenomenex Luna C18色谱柱(250 mm×4.60 mm,5 μm),以甲醇-10 mmol·L-1乙酸铵为流动相,梯度洗脱,流速1.0 mL·min-1,检测波长254 nm,柱温30℃;采用电喷雾离子源(ESI)正负离子模式检测,质谱扫描m/z 100~1 500。对双黄连注射液的氯仿、乙酸乙酯、正丁醇和水4个溶剂萃取部位的化学成分进行分析。结果: 利用多级质谱信息,结合对照品对照及文献数据分析,初步确定了注射液中22个成分的结构,包括3种糖类成分,3种奎宁酸类成分,4种苯乙醇苷类成分,6种木脂素类成分,3种黄酮苷类成分,1种三萜皂苷类成分和2种其他类成分。结论: HPLC-DAD-ESI-MSn联用技术对于中药注射液物质基础的研究有较好的应用价值。
-----英文摘要:---------------------------------------------------------------------------------------
Objective: To analyze the chemical constituents of Shuanghuanglian injection by HPLC-DAD-ESI-MSn.Methods: The chromatography separation was performed on a Phenomenex Luna C18 column(250 mm×4.60 mm,5 μm)maintained at 30℃.Methanol and 10 mmol·L-1 ammonium acetate were used as the mobile phase in gradient elution at a flow rate of 1.0 mL·min-1. Electrospray ionization source was used and the MS scanning was set at the range of m/z 100-1 500. The components in the extrations of chloroform, ethyl acetate, n-butanol and water in Shuanghuanglian injection were detected at 254 nm and positive and negative mode.Results: Based elution at a flow rate of 1.0 mL·min-1 on their MSn fragmentation pattern information,22 compounds including three carbohydrates, three quinic acids, four phenylethanoids, six lignans, three flavonoids, one saponin and two other ingredients were primarily identified by comparing with reference standards and reference data.Conclusion: HPLC-DAD-ESI-MSn technology was applicable for the study of material base of traditional Chinese medicine injection.
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[1] 吕本强,张永勇,罗佳波.双黄连粉针剂的化学成分研究[J].时珍国医国药,2007,18(5):1113 Lǚ BQ,ZHANG YY,LUO JB.Studies on chemical constituents from Shuanghuanglian injection[J].Lishizhen Med Mater Med Res,2007,18(5):1113
[2] 吕本强,杨常成,张贞良,等.双黄连粉针剂化学成分进一步研究[J].解放军药学学报,2009,25(3):225 Lǚ BQ,YANG CC,ZHANG ZL,et al.Further studies on chemical constituents of Shuanghuanglian injection[J].Pharm J Chin PLA,2009,25(3):225
[3] 吕本强,罗佳波.双黄连粉针剂中黄酮类化学成分的研究[J].中成药,2007,29(4):55 Lǚ BQ,LUO JB.Flavonoids in Shuanghuanglian injection[J].Chin Tradit Pat Med,2007,29(4):55
[4] 钮旭升,闫海霞,高慧媛,等.双黄连粉针中抗病毒部位的活性与化学成分研究[J].中国现代中药,2006,8(1):16 NIU XS,YAN HX,GAO HY,et al.Studies on the antivirus activity and chemical constituents from Shuanghuanglian injection powder[J].Mod Chin Med,2006,8(1):16
[5] 张加余,乔延江,张倩,等.液质联用技术在天然产物结构鉴定中的应用进展[J].药物分析杂志,2013,33(2):349 ZHANG JY,QIAO YJ,ZHANG Q,et al.Progress on application of LC-MS technology in structural identification of the natural products[J].Chin J Pharm Anal,2013,33(2):349
[6] 王征,CLIFFORD MN.LC-MSn比较分析三种传统中草药中绿原酸及其衍生物组分[J].药学学报,2008,43(2):185 WANG Z,CLIFFORD MN.Comparison of the profiles of chlorogenic acids and their derivatives from three Chinese traditional herbs by LC-MSn[J].Acta Pharm Sin,2008,43(2):185
[7] 罗奇志,罗佳波,王有志.高效液相色谱-电喷雾串联四极杆质谱定性分析双黄连粉针中化学成分及其药味归属[J].药学学报,2009,44(12):1391 LUO QZ,LUO JB,WANG YZ.Qualitative analysis of the main chemical constituents of Shuanghuanglian injection powder and their origin by HPLC-ESI/MS/MS spectrometry[J].Acta Pharm Sin,2009,44(12):1391
[8] 刘廷,狄留庆,彭琳秀,等.UPLC-MS/MS同时测定双黄连口服液中17种有效成分[J].中草药,2015,46(22):3357 LIU T,DI LQ,PENG LX,et al.Simultaneous determination of 17 major components of Shuanghuanglian oral liquid by UPLC-MS/MS[J].Chin Tradit Herb Drugs,2015,46(22):3357
[9] 李文春,孙永慧,解黎雯,等.HPLC同时测定双黄连粉针剂中15种成分的含量[J].中国新药杂志,2014,23(22):2614 LI WC,SUN YH,XIE LW,et al.Simultaneous determination of fifteen components in Shuanghuanglian powder for injection by HPLC[J].Chin J New Drugs,2014,23(22):2614
[10] HAN J,YE M,GUO H,et al.Analysis of multiple constituents in a Chinese herbal preparation Shuanghuanglian oral liquid by HPLC-DAD-ESI-MSn[J].J Pharm Biomed Anal,2007(44):430
[11] GUO H,LIU AH,YE M,et al.Characterization of phenolic compounds in the fruits of Forsythia suspensa by high-performance liquid chromatography coupled with electrospray ionization tandem mass spectrometry[J].Rapid Commun Mass Spectrom,2007,21:715
[12] WANG FN,MA ZQ,LIU Y,et al.New phenylethanoid glycosides from the fruits of Forsythia suspense(Thunb.)Vahl.[J] Molecules,2009,14:1324
[13] YAMAMOTO H,YOSHIDA K,KONDO Y,et al.Production of cornoside in Abeliophyllum distichum cell suspension cultures[J] Phytochemistry,1998,48(2):273
[14] 吴立军.天然药物化学[M]北京:人民卫生出版社,2004 WU LJ.Medicinal Chemistry of Natural Products[M].Beijing:People's Medical Publishing House,2004
[15] 李凡,易世红,赵春艳,等.双黄连粉针剂抗病毒作用[J].中草药,2002,33(1):52 LI F,YI SH,ZHAO CY,et al.Studies on antivirus effect of Shuanghuanglian injection[J].Chin Tradit Herb Drug,2002,33(1):52
[16] 莫红缨,赖克方,江永南,等.双黄连及其拆方抗呼吸道合胞病毒作用的药效学研究[J].中国中医基础医学杂志,2005,11(3):194 MO HY,LAI KF,JIANG YN,et al.Anti-RSV effects of Shuanghuanglian and its disassembled prescriptions[J].Chin J Basic Med Tradit Chin Med,2005,11(3):194
[17] 高春联,苗明三.双黄连注射液药理与临床研究分析[J].时珍国医国药,2010,21(12):3066 GAO CL,MIAO MS.Analysis of pharmacology and clinical research of Shuanghuanglian injection[J].Lishizhen Med Mater Med Res,2010,21(12):3066
[18] 高玉敏,王名洲,王建平,等.金银花化学成分的研究[J].中草药,1995,26(11):568 GAO YM,WANG MZ,WANG JP,et al.Studies on the chemical constituents of Japanese Honeysuckle(Lonicera japonica)[J].Chin Tradit Herb Drugs,1995,26(11):568
[19] 娄红祥,郎伟君,吕木坚.金银花中水溶性化合物的分离与结构确定[J].中草药,1996,27(4):195 LOU HX,LANG WJ,Lü MJ,et al.Water soluble constituents from Japanese Honeysuckle(Lonicera japonica)[J].Chin Tradit Herb Drugs,1996,27(4):195
[20] 马双成,毕培曦,黄荣春,等.金银花药材中抗呼吸道病毒感染的咖啡酰奎宁酸类成分的定量研究[J].药物分析杂志,2005,25(7):751 MA SC,BI PX,HUANG RC,et al.Determination of the antiviral caffeoyl quinie acids isolated from Lonicera japonica Thunb.[J].Chin J Pharm Anal,2005,25(7):751
[21] 马双成,刘燕,毕培曦,等.金银花药材中抗呼吸道病毒感染的环烯醚萜苷类成分的定量研究[J].药物分析杂志,2006,26(8):1039 MA SC,LIU Y,BI PX,et al.Antiviral activities of iridoids isolated from Lonicera japonica Thunb.[J].Chin J Pharm Anal,2006,26(8):1039
[22] 赵国玲,刘佳佳,林丹,等.金银花化学成分及药理研究进展[J].中成药,2002,24(12):973 ZHAO GL,LIU JJ,LIN D,et al.Studies on the chemical constituents in Flos Lonicerae[J].Chin Tradit Pat Med,2002,24(12):973
[23] 刘东雷,徐绥绪,李会轻,等.连翘中的木脂素单糖苷[J].沈阳药科大学学报,1997,14(3):197 LIU DL,XU SX,LI HQ,et al.Lignan glucosides of Forsythia Suspensa Vahl.[J].J Shenyang Pharm Univ,1997,14(3):197
[24] 刘悦,宋少江,徐绥绪,等.连翘化学成分研究[J].沈阳药科大学学报,2003,20(2):101 LIU Y,SONG SJ,XU SX,et al.Study on the chemical constituents of the fruits of Forsythia suspense(Thunb.)Vahl[J].J Shenyang Pharm Univ,2003,20(2):101
[25] 张海燕.连翘化学成分及药理活性的研究进展[J].中药材,2000,23(10):657 ZHANG HY.Advances in research on chemical constituents and pharmacological activities of Fructus Forsythiae[J].J Chin Med Mater,2000,23(10):657
[26] 刘大伟,闫广利,方圆.UPLC-ESI-TOF/MS应用于黄芩化学成分的快速分析[J].中医药信息,2012,29(4):20 LIU DW,YAN GL,FANG Y,et al.Utility of UPLC-ESI-TOF/MS for rapid analysis of the constituents in Scutellariae Radix[J].Inf Tradit Chin Med,2012,29(4):20
[27] 潘飞,冯毓秀.黄芩研究进展[J].天然产物研究与开发,1994,6(2):61 PAN F,FENG YX.Studies on Radix Scutellariae[J].Nat Prod Res Dev,1994,6(2):61
[28] 杨忻,孟庆刚.黄芩解热化学成分述评[J].中华中医药学刊,2009,27(6):1183 YANG X,MENG QG.Reducing fever chemistry composition study of Scutellaria[J].Chin Arch Tradit Chin Med,2009,27(6):1183
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