太白蓼的高效液相色谱特征图谱研究

目的:建立太白蓼的高效液相色谱特征图谱,用于其质量控制。方法:采用HPLC法梯度洗脱,检测波长280 nm,以甲醇-乙腈(60:40)为流动相A,以0.5%甲酸溶液为流动相B,流速1.0 mL·min^-1,以咖啡酸为参照物计算10批样品共有峰相对保留时间;采用超高效液相色谱串联四极杆飞行时间质谱法(UPLC/Q-TOF-MS法)对太白蓼进行鉴定,并在特征图谱中予以指认。结果:检出8个共有峰,峰面积均大于10 000,通过质谱鉴定确认了其中3个共有峰(绿原酸、咖啡酸、表儿茶素),在质谱鉴定的基础上遴选咖啡酸峰为参照峰,特征峰与参照峰相对保留时间的RSD均小于5%。结论:该特征图谱可用于太白蓼药材鉴别及质量控制,并能区别其类似的混淆品种珠芽蓼、圆穗蓼。

Objective:To establish an HPLC specific chromatograms of Polygonum taipaishanense Kung,so as to control the drug quality.Methods: HPLC gradient elution was adopted for the study.The detection wavelength was 280 nm,the mobile phase of methanol-acetonitrile(60:40)-0.5% formic acid with the flow rate of 1.0 mL·min^-1,and caffeic acid was applied as a reference to calculate peak relative retention time of total product for 10 batches.The results were analyzed on the Polygonum taipaishanense Kung UPLC/Q-TOF MS,and the specific chromatograms were identified.Results:Eight common peaks with area greater than 10 000 were detected.On the basis of mass spectrum identification results,the RSD of relative retention time for both peaks and reference peak were less than 5%.Chlorogenic acid,caffeic acid and epicatchin were identified as Polygonum taipaishanense Kung proposed compounds.Conclusion:These HPLC specific chromatograms can be used for the determination of the Polygonum taipaishanense Kung crude drug and quality control,as well as to distinguish Polygonum taipaishanense Kung from similar species Polygonum viviparum L and Polygonum macrophyllum D.Don.

[1] Northwest Institute of Botany,Chinese Academy of Sciences(中国科学院西北植物研究所).Flora of Qinling(秦岭植物志)[M].Beijing(北京):Science Press(科学出版社),1981:163
[2] WU ZH(吴振海),FU Q(傅青),CHEN SW(陈书文).Shaanxi Chinese herbal medicine(陕西特有的中草药)[J].Chin Pharm J(中国药学杂志),1991,26(11):654
[3] LI YL(李映丽),LV JX(吕居娴),SU YF(苏艳芳).Pharmacognosy studies of Polygonum taipaishanense Kung(太白蓼的生药学研究)[J].J Xi'an Med Univ(西安医科大学学报),1995,16(3):298
[5] SONG XM(宋小妹),LIU HJ(刘海静).The research and application of Taibai Qiyao(太白七药研究与应用)[M].Beijing(北京):People's Medical Publishing House(人民卫生出版社),2011:314
[6] LUO DQ(罗定强),HUANG Y(黄艳),FAN BJ(樊宝娟),et al.Quality atandard of Polygonum macrophyllum D.Don(白蝎子七的质量标准)[J].Anhui Med Pharm J(安徽医药),2013,17(11):1856
[7] DI YL(邸云龙).Study of Quality Standards on the Polygonum taipaishanense Kung(太白蓼质量标准研究)[D].Shaanxi(陕西):Shaanxi University of Chinese Medicine(陕西中医学院),2010
[8] ChP 2010.Vol Ⅰ(中国药典2010年版.一部)[S].2010:50
[9] LIANG B(梁波).Studies on the Chemical Constituents of Two Species of Herb Plant Growing in Taibai Mountains(陕西太白山两种野生药用植物化学成分的研究)[D].Shaanxi(陕西):Shaanxi Normal University(陕西师范大学),2007
[10] QUE S(确生),ZHENG SZ(郑尚珍),MA XM(马雪梅).Studies on the chemical constituents of Polygomum viviparum L.(蝎子七化学成分的研究)[J].J Northwest Normal Univ:Nat Sci(西北师范大学学报:自然科学版),2003,39(4):51
[11] CHENG QF(程茜菲),LIU YH(刘银环),XU MM(许苗苗).HPLC fingerprint of the decoction pieces of Salvia miltiorrhiza(丹参饮片HPLC指纹图谱研究)[J].Northwest Pharm J(西北药学杂志),2013,28(6):556
[12] IBRAHIM M,ABU-REIDAH.HPLC-ESI-Q-TOF-MS for a comprehensive characterization of bioactive phenolic compounds in cucumber whole fruit extract[J].Food Res Int,2011,46:108
[13] CAPRIOTTI AL,CAVALIERE C,CRESCENZI C,et al.Comparison of extraction methods for the identification and quantification of polyphenols in virgin olive oil by ultra-HPLC-QTOF mass spectrometry[J].Food Chem,2014,158:392
[14] FERRERES F,GROSSO C,GIL-IZQUIERDO A,et al.HPLC-DAD-ESI/MSⁿ analysis of phenolic compounds for quality control of Grindelia robusta Nutt.and bioactivities[J].J Pharm Biomed Anal,2014,94:163
[15] QI LW,CHEN CY,LI P.Structural characterization and identification of iridoid glycosides,saponins,phenlic acids and flavonids in Flos Lonicerae Japonicae by a fast liquid chromatography method with diode-array detection and time-of-flight mass spectrometry[J].Rapid Commun Mass Spectrom, 2009,23(19):3227