鹅不食草液相色谱指纹图谱及化学成分表征
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摘要
目的:建立鹅不食草的HPLC指纹图谱,并对其化学成分进行表征。方法:指纹图谱采用Alltima~(TM)C_(18)色谱柱(250 mm×4.6 mm,5μm),柱温为35℃,流动相为乙腈-0.2%磷酸溶液,梯度洗脱;流速为1.0 m L/min;检测波长为290 nm,进样量为20μL。成分表征采用UPLC-QTOF-MS分析,Waters ACQUITY HSS T3(2.1 mm×100 mm,1.8μm)色谱柱,0.1%甲酸乙腈(A)-0.1%甲酸水(B)梯度洗脱,ESI离子源,正离子与负离子模式下采集数据。结果:通过12批鹅不食草的HPLC指纹图谱分析,确定了13个特征峰,12批样品的相似度在0.837~0.997之间;UPLC-QTOF-MS鉴别出26个化学成分,其中Dulcoside A、Kaurane pentanedioic acid derivative及3’,4’-didesulphatedcarboxyatractyloside等二萜苷类化合物系首次在鹅不食草药材中发现。结论:本研究建立的HPLC指纹图谱和化学成分表征信息具有"全息"特征,可为鹅不食草药材整体质量评价提供科学依据。
Objective: To establish chromatographic fingerprint and investigate chemical profile of Centipedae Herba. Methods: The HPLC fingerprint was established on an Alltima~(TM)C_(18) column( 250 mm ×4. 6 mm,5 μm),and the column temperature was 35 ℃. The mobile phase consisted of acetonitrile-0. 2% phosphoric acid in gradient elution and the flow rate was 1. 0 m L/min. The detection wavelength was 290 nm and the injection volume was 20 μL. The chemical profile was studied by UPLC-QTOF-MS analysis,which was conducted on a Waters ACQUITY HSS T3( 2. 1 mm × 100 mm,1. 8 μm). The mobile phase was consisted of solvent A( acetonitrile containing 0. 1% formic acid) and solvent B( 0. 1%formic acid in water). The MS spectra were acquired in both positive and negative ion mode. Results:The HPLC fingerprint of twelve batches of Centipedae Herba was established with thirteen common peaks and the similarity of twelve batches was 0. 837-0. 997. Twenty-six compounds were tentatively identified,with diterpenoid glycosides like Dulcoside A,Kaurane pentanedioic acid derivative and 3 ',4 '-didesulphatedcarboxyatractyloside first reported in Centipedae Herba. Conclusion: The results indicate that the established fingerprint and chemical profile information with holistic characters could provide more comprehensive reference for quality evaluation of Centipedae Herba.
Objective: To establish chromatographic fingerprint and investigate chemical profile of Centipedae Herba. Methods: The HPLC fingerprint was established on an Alltima~(TM)C_(18) column( 250 mm ×4. 6 mm,5 μm),and the column temperature was 35 ℃. The mobile phase consisted of acetonitrile-0. 2% phosphoric acid in gradient elution and the flow rate was 1. 0 m L/min. The detection wavelength was 290 nm and the injection volume was 20 μL. The chemical profile was studied by UPLC-QTOF-MS analysis,which was conducted on a Waters ACQUITY HSS T3( 2. 1 mm × 100 mm,1. 8 μm). The mobile phase was consisted of solvent A( acetonitrile containing 0. 1% formic acid) and solvent B( 0. 1%formic acid in water). The MS spectra were acquired in both positive and negative ion mode. Results:The HPLC fingerprint of twelve batches of Centipedae Herba was established with thirteen common peaks and the similarity of twelve batches was 0. 837-0. 997. Twenty-six compounds were tentatively identified,with diterpenoid glycosides like Dulcoside A,Kaurane pentanedioic acid derivative and 3 ',4 '-didesulphatedcarboxyatractyloside first reported in Centipedae Herba. Conclusion: The results indicate that the established fingerprint and chemical profile information with holistic characters could provide more comprehensive reference for quality evaluation of Centipedae Herba.
引文
[1]国家药典委员会.中华人民共和国药典(一部)[S].北京:中国医药科技出版社,2015:347.
[2]曹俊岭,李国辉.鹅不食草化学成分研究[J].中国中药杂志,2012,37(15):2301-2303.
[3]刘宇,杨艳芳,吴和珍,等.RP-HPLC法测定鹅不食草中短叶老鹳草素的含量[J].中药材,2005,28(6):473-474.
[4]陈惠红,黄婳,项小珍.鹅不食草总黄酮的含量测定方法研究[J].药物研究,2008,17(21):9-10.
[5]陈琦,王尚.鹅不食草总有机酸的提取与分析[J].中国现代药物应用,2010,4(18):10-11.
[6]梁慧,邓洁薇,杨运云.高效液相色谱-质谱法对癍痧凉茶的化学成分鉴定及指纹图谱研究[J].分析测试学报,2014,33(2):144-149.
[7]聂平,肖炳焱,罗晖明,等.超高效液相色谱-质谱联用技术在中药指纹图谱中的应用[J].中南药学,2013,11(7):524-527.
[8]CHAN C O,JIN D P,DONG N P,et al.Qualitative and quantitative analysis of chemical constituents of Centipeda minima by HPLC-QTOF-MS&HPLC-DAD[J].J Pharm Biomed Anal,2016,125:400-407.
[9]杨艳芳,张炳武,闫斌,等.鹅不食草正丁醇部位化学成分研究[J].时珍国医国药,2013,24(10):2358-2359.
[10]曹俊岭,李国辉.鹅不食草化学成分研究[J].中国中药杂志,2012,37(15):2301-2303.
[11]朱艳平.鹅不食草化学成分及抗肿瘤活性研究[D].武汉:湖北中医药大学,2012.
[12]WU P,LI X G,LIANG N,et al.Two new sesquiterpene lactones from the supercritical fluid extract of Centipeda minima[J].J Asian Nat Prod Res,2012,14(6):515-520.
[13]WU P,SU M X,WANG Y,et al.Supercritical fluid extraction assisted isolation of sesquiterpene lactones with antiproliferative effects from Centipeda minima[J].Phytochemistry,2012,76:133-140.
[14]MOLINA-CALLE M,PRIEGO-CAPOTE F,LUQUE DE CASTRO M D.Characterization of Stevia leaves by LC-QTOF MS/MS analysis of polar and non-polar extracts[J].Food chemistry,2017,219:329-338.
[15]ZHENG Q A,ZHANG Y J,LI H Z,et al.Steroidal saponins from fresh stem of Dracaena cochinchinensis[J].Steroids,2004,69(2):111-119.
[16]CELIA B B,MARIANO S C,BALDOMERO E,et al.ent-Kaurene Glycosides from Ageratina cylindrica[J].J Nat Prod,2015,78(11):2580-2587.
[17]DUBIOS G E,ALTO P,CALIF.Rebaudioside analogs:United States Patent:4353889[P].1982-10-12.
[18]PIACENTE S,PIZZA C,TOMMASIT N D,et al.Sesquiterpene and diterpene glycosides from Xanthium spinosum[J].Phytochemistry,1996,41(5):1357-1360.
[2]曹俊岭,李国辉.鹅不食草化学成分研究[J].中国中药杂志,2012,37(15):2301-2303.
[3]刘宇,杨艳芳,吴和珍,等.RP-HPLC法测定鹅不食草中短叶老鹳草素的含量[J].中药材,2005,28(6):473-474.
[4]陈惠红,黄婳,项小珍.鹅不食草总黄酮的含量测定方法研究[J].药物研究,2008,17(21):9-10.
[5]陈琦,王尚.鹅不食草总有机酸的提取与分析[J].中国现代药物应用,2010,4(18):10-11.
[6]梁慧,邓洁薇,杨运云.高效液相色谱-质谱法对癍痧凉茶的化学成分鉴定及指纹图谱研究[J].分析测试学报,2014,33(2):144-149.
[7]聂平,肖炳焱,罗晖明,等.超高效液相色谱-质谱联用技术在中药指纹图谱中的应用[J].中南药学,2013,11(7):524-527.
[8]CHAN C O,JIN D P,DONG N P,et al.Qualitative and quantitative analysis of chemical constituents of Centipeda minima by HPLC-QTOF-MS&HPLC-DAD[J].J Pharm Biomed Anal,2016,125:400-407.
[9]杨艳芳,张炳武,闫斌,等.鹅不食草正丁醇部位化学成分研究[J].时珍国医国药,2013,24(10):2358-2359.
[10]曹俊岭,李国辉.鹅不食草化学成分研究[J].中国中药杂志,2012,37(15):2301-2303.
[11]朱艳平.鹅不食草化学成分及抗肿瘤活性研究[D].武汉:湖北中医药大学,2012.
[12]WU P,LI X G,LIANG N,et al.Two new sesquiterpene lactones from the supercritical fluid extract of Centipeda minima[J].J Asian Nat Prod Res,2012,14(6):515-520.
[13]WU P,SU M X,WANG Y,et al.Supercritical fluid extraction assisted isolation of sesquiterpene lactones with antiproliferative effects from Centipeda minima[J].Phytochemistry,2012,76:133-140.
[14]MOLINA-CALLE M,PRIEGO-CAPOTE F,LUQUE DE CASTRO M D.Characterization of Stevia leaves by LC-QTOF MS/MS analysis of polar and non-polar extracts[J].Food chemistry,2017,219:329-338.
[15]ZHENG Q A,ZHANG Y J,LI H Z,et al.Steroidal saponins from fresh stem of Dracaena cochinchinensis[J].Steroids,2004,69(2):111-119.
[16]CELIA B B,MARIANO S C,BALDOMERO E,et al.ent-Kaurene Glycosides from Ageratina cylindrica[J].J Nat Prod,2015,78(11):2580-2587.
[17]DUBIOS G E,ALTO P,CALIF.Rebaudioside analogs:United States Patent:4353889[P].1982-10-12.
[18]PIACENTE S,PIZZA C,TOMMASIT N D,et al.Sesquiterpene and diterpene glycosides from Xanthium spinosum[J].Phytochemistry,1996,41(5):1357-1360.