胡黄连苷-Ⅱ原料药特征图谱研究及有关物质测定

目的: 采用高效液相色谱法建立胡黄连苷-Ⅱ原料药特征图谱并测定有关物质。方法: 采用Kromasil 100-5 C₁₈色谱柱(250 mm×4.6 mm,5 μm),流动相为乙腈-0.2%乙酸溶液(15.5:84.5),流速1 mL·min^-1,检测波长264 nm,柱温30℃,进样量10 μL。结果: 建立了胡黄连苷-Ⅱ原料药的特征图谱,样品特征图谱有5个特征峰,仅有3个有关物质的面积百分比在0.1%以上,主成分与有关物质分别在本文色谱条件下分离良好。胡黄连苷-Ⅱ 的线性范围为117.92~1 887 μg·mL^-1(r=0.999 9,n=5);平均回收率(n=6)为98.58%。结论: 本方法准确,重复性好,可作为胡黄连苷-Ⅱ原料药质量控制时测定有关物质的方法。

Objective: To develop an HPLC method for determination of the related substances in raw material drug of picroside-Ⅱ. Methods: The analysis was conducted by RP-HPLC using a Kromasil 100-5 C₁₈ column (250 mm×4.6 mm, 5 μm).The mobile phase was acetonitrile-0.2% acetic acid(15.5: 84.5)with a flow rate of 1.0 mL·min^-1.The detection wavelength was 264 nm.The column temperature was 30℃, and the injection volume was 10 μL. Results: The charaeterization chromatograms of the Picroside-Ⅱwas established.Five common peaks were separated in the test sample.Only 3 of the related substances had the area normalization content over 0.1%.The prominent peak and the neighboring subsidiary peak were completely separated by the method.The linear range of picroside-Ⅱ was 117.92-1 887 μg·mL^-1(r=0.999 9, n=5), with an average recovery of 98.58%(n=6). Conclusion: The method is precise and reproducible, which is reliable for the analysis of related substances in raw material drug of picroside-Ⅱ.

[1] SINGH H,GAHLAN P,DUTT S,et al.Why uproot Picrorhiza kurrooa,an endangered medicinal herb[J].Curr Sci,2011,100:1055
[2] WANG H(汪豪),WU JJ(吴佳俊),LIU G(刘戈),et al.Chemical studies on iridoids from Picrorhiza scrophulariiflora(西藏胡黄连中的环烯醚萜类化学成分)[J].Chin J Nat Med(中国天然药物),2006,4(1):36
[3] HAN H(韩华),YIN X(殷鑫),ZHANG TY(张天宇),et al.Advances in the study of Rhizoma Picrorhizae (西藏胡黄连的研究进展)[J].Acta Chin Med Pharmacol(中医药学报),2014,42(2):94
[4] LIU ZC(刘志春).Review on the chemical constituents of Picrorhiza scrophulariiflora Pennell(西藏胡黄连的化学成分研究进展)[J].J Pharm Pract (药学实践杂志),2010,28(5):321
[5] HE XR(何希瑞),LI Q(李倩),ZHANG CL(张春玲),et al.Phytochemical and biological studies on Picrorrhiza scrophularaeflora Pennell(胡黄连化学成分及单体化合物药理活性研究新进展)[J].Global Tradit Chin Med(环球中医药),2012,5(9):708
[6] HOU WB(侯文彬),ZHOU FJ(周福军),SHAN Q(单淇),et al.HPLC characteristic chromatograms of total glucosides in Picrorhiza scrophulariiflora (胡黄连总苷的高效液相色谱特征图谱研究)[J].Drugs Clin(现代药物与临床),2013,28(5):712
[7] XIE MF(谢沐风),LUO XP(罗霞萍),CHEN Ya-mei(陈亚美).How to build the method of the related substance analysis by HPLC(如何建立HPLC法测定有关物质的方法)[J].Drug Stand China(中国药品标准),2002,3(6):6
[8] DI B(狄斌),SU MX(苏梦翔),YANG QQ(杨清清),et al.HPLC determination of diltiazem hydrochloride and related substances in delay-onset sustained-release pellet capsules (HPLC测定盐酸地尔硫延迟缓释微丸胶囊的含量及有关物质检查)[J].Chin J Pharm Anal(药物分析杂志),2008,28(1):65
[9] LI YL(李云兰),NING MY(宁美英),YANG F(杨帆),et al.NP-HPLC determination of titanocene dichloride and its related substances(NP-HPLC法测定二氯二茂钛原料药的含量及有关物质)[J].Chin J Pharm Anal(药物分析杂志),2008,28(1):76