HPLC-MS/MS法测定巴天酸模中7个蒽醌类成分含量
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摘要
目的:采用HPLC-MS/MS法测定巴天酸模中7个蒽醌类成分的含量。方法:采用SB-C_(18)色谱柱(4.6 mm×100 mm,1.8μm),流动相为乙腈(A)-0.1%甲酸水(B)。梯度洗脱程序为:0~8.5 min,95%~95%A;8.5~8.51 min,95%~40%A;8.51~12 min,40%~40%A。流动相流速为0.4 mL/min,柱温为20℃,进样量为10μL。结果:大黄酸、芦荟大黄素在2.5~50 ng/mL,大黄素、大黄素甲醚在10~250 ng/mL,大黄酚在25~1000 ng/mL,大黄素-8-O-葡萄糖苷、大黄素甲醚-8-O-葡萄糖苷在10~500 ng/mL范围内,进样量与峰面积具有良好线性关系(r~2均>0.98)。同时,其平均加样回收率在90.32%~106.75%(n=6)。结论:该方法简便、准确、灵敏,可用于巴天酸模中蒽醌类成分的含量测定。
Objective:To establish a HPLC-MS/MS method for determining the content of seven anthraquinones constituents in Polygonum Rumex Patientia L.Methods:A SB-C_(18) column(4.6mm×100 mm,1.8μm) was used with a mobile phase of acetonitrile(A)-0.1%acetic acid in water(B).The gradient elution program was as follows:0~8.5 min,95%~95%A;8.5~8.51 min,95%~40%A;8.51~12 min,40%~40%A.The column temperature was set at 20 °C.The flow rate was kept at 0.4 mL/min and the sample volume was 10μL.Results:All calibration curves had good linearity(r2>0.98)over the concentration ranges of 2.5-50 ng/mL for rhein and aloe rhein,10-250 ng/mL for emodin and physcion,25~1000 ng/mL for chrysophanol,10~500 ng/mL for emodin-8-O-glucoside and physcion-8-O-glucoside.And the average recoveries were all ranged in 90.32%~106.75%(n=6).Conclusion:The method is simple,accurate and sensitive for the determination of anthraquinones constituents in Polygonum Rumex Patientia L..
Objective:To establish a HPLC-MS/MS method for determining the content of seven anthraquinones constituents in Polygonum Rumex Patientia L.Methods:A SB-C_(18) column(4.6mm×100 mm,1.8μm) was used with a mobile phase of acetonitrile(A)-0.1%acetic acid in water(B).The gradient elution program was as follows:0~8.5 min,95%~95%A;8.5~8.51 min,95%~40%A;8.51~12 min,40%~40%A.The column temperature was set at 20 °C.The flow rate was kept at 0.4 mL/min and the sample volume was 10μL.Results:All calibration curves had good linearity(r2>0.98)over the concentration ranges of 2.5-50 ng/mL for rhein and aloe rhein,10-250 ng/mL for emodin and physcion,25~1000 ng/mL for chrysophanol,10~500 ng/mL for emodin-8-O-glucoside and physcion-8-O-glucoside.And the average recoveries were all ranged in 90.32%~106.75%(n=6).Conclusion:The method is simple,accurate and sensitive for the determination of anthraquinones constituents in Polygonum Rumex Patientia L..
引文
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[13]杜鹃,吴桂芳,刘雅华.RP-HPLC法测定贵阳地区不同采收期土大黄中大黄素及总游离蒽醌含量[J].中草药,1998,29(6):387-388.
[14]Zhu JJ,Zhang CF,Zhang MA,et al.Separation and identification of three epimeric pairs of new C-glucosyl anthrones from Rumex dentatus by on-line high performance liquid chromatography-circular dichroism analysis[J].J Chromatogr A,2010,1217(33):5384-5388.
[15]Gautam R,Srivastava A,Jachak SM.Simultaneous Determination of Naphthalene and Anthraquinone Derivatives in Rumex nepalensis Spreng.Roots by HPLC:Comparison of Different Extraction Methods and Validation[J].Phytochem Analysis,2011,22(2):153-157.
[16]Shia CS,Juang SH,Tsai SY,et al.Metabolism and pharmacokinetics of anthraquinones in Rheum palmatum in rats and ex vivo antioxidant activity[J].Planta medica,2009,75(13):1386-1392.
[2]伊合帕尔·木拉提,艾合买提·买买提,玛依努尔·阿不拉.维吾尔医治疗银屑病108例临床观察[J].中国民族医药杂志,2005(3):3.
[3]Chang CH,Lin CC,Yang JJ,et al.Anti-inflammatiry effects of emodin from ventilago leiocarpa[J].Am J Chin Med,1996,24(2):139-142.
[4]王莉,旺姆,桑姆.尼泊尔酸模根中活性蛋白—凝集素特性初探[J].中国野生植物资源,2004(4):48-49.
[5]张燕,李治建,夏木西努尔·肖盖提,等.土大黄化学成分及药理作用研究进展[J].中药药理与临床,2012,28(3):173-176.
[6]El-Kader AMA,El-Mawla AMAA,Mohamed MH,et al.Phytochemical and biological studies of Emex spinosa(L.)Campd.growing in Egypt[J].Bull Pharm Sci,2006,29:328-347.
[7]Litvinenko YA,Muzychkina RA.Phytochemical investigation of biologically active substances in certain Kazakhstan Rumex species.1[J].Chem Nat Compd,2003,39(5):446-449.
[8]Wegiera M,Smolarz HD,Wianowska D,et al.Anthracene derivatives in some species of Rumex L.genus[J].Acta Soc Bot Pol,2007,76(2):103-108.
[9]Liu SY,Sporer F,Wink M,et al.Anthraquinones in Rheum palmatum and Rumex dentatus(Polygonaceae),and phorbol esters in Jatropha curcas(Euphorbiaceae)with molluscicidal activity against the schistosome vector snails Oncomelania,Biomphalaria and Bulinus[J].Trop Med Int Health,1997,2(2):179-188.
[10]Guo SY,Feng B,Zhu RN,et al.Preparative Isolation of Three Anthraquinones from Rumex japonicus by High-Speed CounterCurrent Chromatography[J].Molecules,2011,16(2):1201-1210.
[11]王克英.HPLC测定土大黄中大黄素的含量[J].中国中医药信息杂志,2003,10(9):34-35.
[12]原源,陈万生,张汉明,等.HPLC法测定酸模属植物根中蒽醌类成分的含量[J].第二军医大学学报,2000,21(10):952-954.
[13]杜鹃,吴桂芳,刘雅华.RP-HPLC法测定贵阳地区不同采收期土大黄中大黄素及总游离蒽醌含量[J].中草药,1998,29(6):387-388.
[14]Zhu JJ,Zhang CF,Zhang MA,et al.Separation and identification of three epimeric pairs of new C-glucosyl anthrones from Rumex dentatus by on-line high performance liquid chromatography-circular dichroism analysis[J].J Chromatogr A,2010,1217(33):5384-5388.
[15]Gautam R,Srivastava A,Jachak SM.Simultaneous Determination of Naphthalene and Anthraquinone Derivatives in Rumex nepalensis Spreng.Roots by HPLC:Comparison of Different Extraction Methods and Validation[J].Phytochem Analysis,2011,22(2):153-157.
[16]Shia CS,Juang SH,Tsai SY,et al.Metabolism and pharmacokinetics of anthraquinones in Rheum palmatum in rats and ex vivo antioxidant activity[J].Planta medica,2009,75(13):1386-1392.