HPLC法测定羚翘解毒片中绿原酸含量.docVIP

HPLC法测定羚翘解毒片中绿原酸含量 　　[摘要] 目的:建立高效液相色谱法测定羚翘解毒片中绿原酸含量的方法。方法:采用Kromasil-C18(4.6 mm×200 mm;5 μm)色谱柱,流动相:甲醇-水-冰醋酸-三乙胺(18∶85∶1∶0.3);流速:1.0 ml/min;检测波长:324 nm。结果:绿原酸在17.22～172.20 μg/ml(r=0.999 8)范围内线性关系良好,平均回收率为98.23%,RSD=0.71%(n=6)。结论:本方法操作简便,准确度高,重现性好,可作为该产品质量控制的方法。 　　[关键词] HPLC;羚翘解毒片;绿原酸;含量测定 　　[中图分类号] R927.2[文献标识码] A [文章编号] 1673-7210(2010)06(a)-067-02 　　 　　Content determination of Chlorogenic acid in Lingqiao Jiedu Tablets by HPLC 　　ZHANG Xiuli1, LUO Jing2 　　(1.Institute for Drug Control in Chaoyang City, Chaoyang 122000, China; 2. Institute for Drug Control in Fushun City, Fushun 113006, China) 　　[Abstract] Objective: To establish a method for the content determination of chlorogenic acid in Lingqiao Jiedu Tablets by HPLC. Methods: The Kromasil-C18 (4.6 mm×200 mm, 5 μm) column was used. The mobile phases consisted of methanol, water, acetic acid and triethylamine (18∶85∶1∶0.3), the flow rate was 1.0 ml/min and the detection wavelength was at 324 nm. Results: The linear range of Chlorogenic acid was at 17.22-172.20 μg/ml (r=0.999 8), the average recovery was 98.23% with a RSD of 0.71% (n=6). Conclusion: The method is fast, reliable, accurate and can be used in the quality control of chlorogenic acid in Lingqiao Jiedu Tablets. 　　[Key words] HPLC; Lingqiao Jiedu Tablets; Chlorogenic acid; Content determination 　　 　　羚翘解毒片由羚羊角粉、金银花、连翘、荆芥穗等12味药制备而成的片剂,具有辛凉解表、清热解毒之功效。由于原标准过于简单,无含量测定方法,为了提高本品的内在质量,增强标准的约束能力,笔者采用高效液相色谱法测定金银花中绿原酸的含量,现报道如下: 　　1 仪器与试药 　　Sp8810高效液相色谱仪,N2010色谱工作站, Spectra100紫外检测器。绿原酸对照品(中国药品生物制品检定所,批号:110753-200212);供试品(批号:7124088、8015449、7082049,市售);甲醇(色谱纯),水(重蒸馏水),冰醋酸、三乙胺(分析纯)。 　　2 方法与结果 　　2.1 色谱条件与系统适用性试验 　　色谱柱Kromasil-C18(4.6 mm×200 mm,5 μm);流动相:甲醇-水-冰醋酸-三乙胺(18∶85∶1∶0.3);流速:1.0 ml/min;柱温:室温;检测波长:324 nm;,进样量:20 μl。在此条件下,理论板数按绿原酸计算不低于3 000,分离度大于1.5。色谱图见图1。 　　2.2 溶液的制备 　　2.2.1 对照品溶液的制备精密称取五氧化二磷真空干燥至恒重的绿原酸对照品8.61 mg,置25 ml棕色量瓶中,加50%甲醇溶解并稀释至刻度,摇匀,作为对照品贮备液。再精密吸取对照品贮备液3 ml,置10 ml棕色量瓶中,加50%甲醇稀释至刻度,摇匀,即得绿原酸对照品溶液。 　　2.2.2 供试品溶液的制备取重量差异项下的样品研细,取约0.25 g