中药女贞子饮片中8个成分的含量比较研究
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摘要
目的:针对不同来源女贞子和酒女贞子饮片中8个成分(红景天苷、酪醇、特女贞苷、木犀草苷、木犀草素、芹菜素、齐墩果酸、熊果酸)建立高效液相色谱含量测定方法,并对女贞子、酒女贞子饮片及水煎煮前后所测成分的含量进行比较,为其质量标准提高和临床应用提供依据。方法:采用液相色谱法,使用Agilent Prep-C18(4.6 mm×250 mm,5μm)色谱柱,以乙腈(A)-0.02%磷酸水溶液(B)为流动相,梯度洗脱(0~5 min,5%A→10%A;5~15 min,10%A;15~60 min,10%A→33%A;60~65 min,33%A→90%A;65~75 min,90%A;75~80 min,100%A),流速1 m L·min-1,检测波长224 nm(测定红景天苷、酪醇、特女贞苷)、349 nm(测定木犀草苷、木犀草素、芹菜素)、206 nm(测定齐墩果酸、熊果酸),柱温25℃。结果:建立的8个成分含量测定方法简便、可行;女贞子、酒女贞子饮片中红景天苷、酪醇、木犀草素和芹菜素的含量存在显著性差异;2种饮片的水煎液中红景天苷、酪醇、特女贞苷、木犀草苷可检出,且变化明显。结论:木犀草素和芹菜素可以用于饮片的鉴别,红景天苷、酪醇、特女贞苷、木犀草苷具有特征性,可用于女贞子、酒女贞子饮片的质量评价。
Objective: To establish an HPLC method for determination of eight components( salidroside,tyrosol,specnuezhenide,luteolin-7-O-glucoside,luteolin,apigenin,oleanolic acid and ursolic acid) in Ligustri Lucidi Fructus and wine-baked Ligustri Lucidi Fructus pieces from different sources,and compare the content in the water decoction,Ligustri Lucidi Fructus,so as to provide a foundation for the improvement of quality standard and clinical application. Methods: The analysis was performed on an Agilent Prep-C18( 4. 6 mm × 250 mm,5 μm) column. The mobile phase was acetonitrile( A)-0. 02% phosphoric acid aqueous( B) with gradient elution mode( 0-5 min,5%A→10% A; 5-15 min,10% A; 15-60 min,10% →33% A; 60-65 min,33% A→90% A; 65-75 min,90% A; 75-80 min,100% A),at a flow rate of 1 m L·min-1. The detection was set at 224 nm for salidroside,tyrosol,and specnuezhenide; 349 nm for luteolin-7-O-glucoside,luteolin,and apigenin; 206 nm for oleanolic acid and ursolic acid.The column temperature was controlled at 25 ℃. Results: The HPLC determination method established for eight components is easy and feasible; the content of salidroside,tyrosol,luteolin and apigenin were significantly different between Ligustri Lucidi Fructus and wine-baked Ligustri Lucidi Fructus pieces; salidroside,tyrosol,specnuezhenide and luteolin-7-O-glucoside could be detected and obviously changed in the water decoction of two kinds of pieces.Conclusion: Luteolin and apigenin can be used for identification of two pieces. Salidroside,tyrosol,specnuezhenide and luteolin-7-O-glucoside are characteristic. The HPLC determination method established in the study can be used for the quality control of Ligustri Lucidi Fructus and wine-baked Ligustri Lucidi Fructus pieces.
Objective: To establish an HPLC method for determination of eight components( salidroside,tyrosol,specnuezhenide,luteolin-7-O-glucoside,luteolin,apigenin,oleanolic acid and ursolic acid) in Ligustri Lucidi Fructus and wine-baked Ligustri Lucidi Fructus pieces from different sources,and compare the content in the water decoction,Ligustri Lucidi Fructus,so as to provide a foundation for the improvement of quality standard and clinical application. Methods: The analysis was performed on an Agilent Prep-C18( 4. 6 mm × 250 mm,5 μm) column. The mobile phase was acetonitrile( A)-0. 02% phosphoric acid aqueous( B) with gradient elution mode( 0-5 min,5%A→10% A; 5-15 min,10% A; 15-60 min,10% →33% A; 60-65 min,33% A→90% A; 65-75 min,90% A; 75-80 min,100% A),at a flow rate of 1 m L·min-1. The detection was set at 224 nm for salidroside,tyrosol,and specnuezhenide; 349 nm for luteolin-7-O-glucoside,luteolin,and apigenin; 206 nm for oleanolic acid and ursolic acid.The column temperature was controlled at 25 ℃. Results: The HPLC determination method established for eight components is easy and feasible; the content of salidroside,tyrosol,luteolin and apigenin were significantly different between Ligustri Lucidi Fructus and wine-baked Ligustri Lucidi Fructus pieces; salidroside,tyrosol,specnuezhenide and luteolin-7-O-glucoside could be detected and obviously changed in the water decoction of two kinds of pieces.Conclusion: Luteolin and apigenin can be used for identification of two pieces. Salidroside,tyrosol,specnuezhenide and luteolin-7-O-glucoside are characteristic. The HPLC determination method established in the study can be used for the quality control of Ligustri Lucidi Fructus and wine-baked Ligustri Lucidi Fructus pieces.
引文
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[2]ZHANG JL(张金玲),WANG XH(王小虎),DENG ZT(邓振涛),et al.Advances in studies on chemical constutuents and pharmacological activities of Fructus Ligustri Lucidi(中药女贞子化学成分及药理作用研究进展)[J].Mod J Integr Tradit Chin West Med(现代中西医结合杂志),2013,22(26):4100
[3]SHI LF(石力夫),CAO YY(曹颖瑛),CHEN HS(陈海生),et al.Separation and identification of two new secoiridoid gylcosides of water-soluble constituents in Fructus Ligustri Lucidi(中药女贞子中水溶性成分二种新裂环环烯醚萜苷的分离和鉴定)[J].Acta Pharm Sin(药学学报),1997,32(6):442
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[6]HUANG XX(黄晓君),YIN ZQ(殷志琦),YE WC(叶文才),et al.Studies on the chemical constituents of Fructus Ligustri Lucidi(女贞子的化学成分研究)[J].China J Chin Mater Med(中国中药杂志),2010,35(7):861
[7]KONG LB,LI SS,LIAO QJ,et al.Oleanolic acid and ursolic acid:novel hepatitis C virus antivirals that inhibit NS5B activity[J].Antiviral Res,2013,98(1):44
[8]ZHANG TF(张廷芳),DUAN YH(段营辉),TU FJ(屠凤娟),et al.A new secoiridoid glucoside in fruits of Ligustrum lucidum(女贞子中一个新的裂环环烯醚萜苷类成分)[J].Chin Tradit Herb Drugs(中草药),2012,43(1):20
[9]SHI KB(史昆波),SHENG ZH(盛振环).Identification of Ligustrum lucidum Ait.by X-Ray diffraction fourier pattern method(女贞子的X射线衍射Fourier指纹图谱鉴定)[J].J Chin Med Mater(中药材),2007,30(6):643
[10]DING X(丁雪),SHI LF(石力夫).Research on HPLC fingerprint of active components in acetic ether extract of Ligustrum lucidum(女贞子乙酸乙酯有效部位群的HPLC指纹图谱研究)[J].Pharm Care Res(药学服务与研究),2010,10(5):368
[11]XU CG(徐长根),LI T(李涛),FU Q(傅强).Preliminary study on fingerprints of Fructus Ligustri Lucidi by HPLC(女贞子药材HPLC指纹图谱的初步研究)[J].Tradit Chin Drug Res Clin Pharmacol(中药新药与临床药理),2005,16(5):368
[12]KONG DP(孔德平),LU LL(陆林玲),QIAN DW(钱大玮),et al.Analysis and evaluation for dynamic accumulation of multicriteria chemical compositions from Ligustrum lucidum Ait.in different mature periods(女贞果实不同成熟期多指标化学成分动态积累的分析与评价)[J].J Nanjing Univ Tradit Chin Med(南京中医药大学学报),2011,27(3):273
[13]WANG D(王丹),LYL(吕亚丽),LIU CS(刘春生),et al.Content determination of total secoiridoid glucosides in Fructus Ligustri Lucidi(女贞子中裂环环烯醚萜总苷的含量测定)[J].Pharm Care Res(药学服务与研究),2012,12(1):52
[14]WANG SS,LUO LJ,LI YQ,et al.Qualitative and quantitative analysis of effective components in Fructus Ligustri Lucidi by near infrared spectroscopy[J].Anal Methods,2013,5(12):3045
[15]FAN YC(范永春),XU XY(徐小燕),YANG YX(杨元勋).Content determination of luteoliin and apigenin in Ligustrum lucidum by HPLC(HPLC法同时测定女贞子中木犀草素和芹菜素的含量)[J].China Pharm(中国药房),2013,24(39):3702
[16]REN HY(任华益).To measure and compare the content of salidroside or P-tyrosol in Fructus Ligustri lucid in Changsha from different months and processings(不同采收月份和不同炮制方法对女贞子中红景天苷和酪醇含量的影响)[J].Anti-tumor Pharm(肿瘤药学),2011,1(2):136
[17]ZHANG L(张丽),CHEN T(陈汀),CAO YD(曹雨诞),et al.Study on content of oleanolic acid and ursolic acid in different processed products and different years of growth of Ligustri Lucidi Fructus(女贞子不同炮制品及不同树龄中齐墩果酸和熊果酸含量研究)[J].Chin J Exp Tradit Med Form(中药实验方剂学杂志),2011,17(1):46
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