摘要
本研究采用高效液相色谱建立了一种简便、灵敏可同时测定刺五加茎中原儿茶酸、L-苯丙氨酸、刺五加苷B、绿原酸、咖啡酸、刺五加苷E和异嗪皮啶含量的方法。采用Welchrom C18色谱柱(250×4.6 mm,5μm),以乙腈-0.1%磷酸水为流动相,流速为1 mL·min~(-1),检测波长为210 nm,柱温为30℃。在55 min内,刺五加茎中7种成分完全分离,样品含量与其对应峰面积Y呈现良好的线性关系(r=0.999 3~0.999 9);平均加样回收率为99.2%~100.7%,RSD为0.72%~1.14%。应用该方法,我们对采收于不同日期的刺五加茎中的七种成分进行了测定,测定结果表明,7种功效成分含量的综合评价指标在11月份较高。本研究建立的多成分HPLC测定方法简便、灵敏、稳定,适合用于刺五加多成分的定量分析和刺五加药材质量控制。
A simple and sensitive HPLC method was established for simultaneous determination of seven compounds( protocatechuic acid,L-phenylalanine,syringin,chlorogenic acid,caffeic acid,eleutheroside E and isopyrazidine) in the stems of Acanthopanax senticosus( Rupr. Maxim.) Harms. The seven compounds were analyzed simultaneously with a Welchrom C18( 250 mm × 4. 6 mm,5 μm) column by gradient elution using 0. 1‰( v/v) phosphoric acid-acetonitrile as the mobile phase at the flow rate of 1. 0 mL/min; The detection wavelength was set at 210 nm,and the column temperture was maintained at 30 ℃. The highest average contents of seven contents were found in A. senticosus stems collected in November. This method was easy to operate and could provide a reference for the quality control of the stem of A. senticosus.
引文
1 Chinese Pharmacopoeia Commission(国家药典委员会).Pharmacopoeia of the People’s Republic of China:Vol I(中华人民共和国药典:第一部)[M].Beijing:China Medical Science Press,2015:206-207.
2 Liu HP(刘和平),Xu Y(许彦),Min JH(闵建华),et al.Content variations of crocin I,crocin II and gardenoside in Gardenia jasminoides var.grandiflora with different harvesting times[J].Nat Prod Res Dev(天然产物研究与开发),2017,29:1333-1338.
3 Yan ZW(闫兆威),Liu JP(刘金平),Lu D(卢丹),et al.A new 3,4-seco-lupane-type triterpenoid from the pulp of Acanthopanax senticosus(Rupr.et Maxim)Harms[J].Nat Prod Res Dev(天然产物研究与开发),2010,24:1523-1527.
4 Li Q,Jia Y,Xu L,et al.Simultaneous determination of protocatechuic acid,syringin,chlorogenic acid,caffeic acid,liriodendrin and isofraxidin in Acanthopanax senticosus Harms by HPLC-DAD[J].Biol Pharm Bull,2006,29:532-534.
5 Huang LZ,Zhao HF,Huang BK,et al.Acanthopanax senticosus:review of botany,chemistry and pharmacology[J].Pharmazue,2011,66:83-97.
6 Zhou X,Zheng C,Huang J,et al.Identification of herb Acanthopanax senticosus(Rupr.Et Maxim.)harms by capillary electrophoresis with electrochemical detection[J].Anal Sci,2007,23:705-711.
7 Khan AK,Rashid R,Fatima N,et al.Pharmacological activities of protocatechuic acid[J].Acta Pol Pharm,2015,72:643-650.
8 Sun H,Liu J,Zhang A,et al.Characterization of the multiple com-ponents of Acanthopanax senticosus stem by ultra HPLC with quadrupole time-of-flight tandem masss pectrometry[J].J Sep Sci,2016,39:496-502.
9 Meng XC(孟祥才),Yan BP(颜丙鹏),Sun H(孙晖),et al.The seasonal accumulating study on effective constituent contents in different sexual types of rhizome and stem of Acanthopanax senticosus[J].Lishizhen Med Mater Med Res(时珍国医国药),2012,23:601-603.
10 Zhang Y(张颖),Yue SQ(岳姝岐),Li RF(李瑞芳),et al.Determination of content of total lignans in the stem of Acanthopanax senticosus[J].Chem Engineer(化学工程师),2016,30:28-30.
11 Zhang CX(张崇禧),Zhang Q(张倩),Cai EB(蔡恩博),et al.HLPC comparison Acanthopanax stems and Acanthopanax sessili florus syringin and isoxapide content[J].Chin Tradit Pat Med(中成药),2010,32:254-256.
12 Zhang CX(张崇禧),Wang TY(王桐玉),Tian X(田芯),et al.The content of syringin and total flavonoids in Acanthopanax senticosus and determined in different harvesting times[J].Chin Tradit Pat Med(中成药),2009,31:82-85.
13 Sun H(孙晖),Sui JT(隋金婷),Meng XC(孟祥才),et al.Study on optimum harvesting period of Acanthopanax senticosus[J].Chin Journal of Trad Mel Sci and Tech(中国中医药科技),2007:225.
14 Huang SD(黄世德).Analysis chemistry:Vol.2(分析化学:下册)[M].Beijing:China Press of Traditional Chinese Medicine,2005:10-12.
15 Pan RC(潘瑞炽).Plant physiology(植物生理学)[M].Beijing:Higher Education Press,2008:136-139.
16 ZHANG BX(张宝香),YANG YM(杨义明),JIANG Y(姜英),et al.Study on the drying rate and saponin content in different tree age and different harvest time of Acanthopanax senticosus[J].Spec Eco Anim and Pln Res(特产研究),2010,2:17.