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[摘要]
目的 建立冠脉通片的质量控制方法。方法 采用TLC法,分别以甲苯-醋酸乙酯-甲酸(15∶2∶1)、乙酸丁酯-甲酸-水(1.3∶1∶1)10 ℃下放置的上层溶液为展开剂对何首乌及淫羊藿进行薄层色谱鉴别;采用气相色谱法,以水杨酸甲酯为内标物,安捷伦DB-WAX毛细管柱(30 m×0.53 mm,1 μm),FID检测器,载气为氮气,柱温为140 ℃,测定冠脉通片中的冰片;采用高效液相色谱法,Dikma-C18色谱柱(250 mm×4.6 mm,5 μm),甲醇-0.5%乙酸(88∶12)为流动相,体积流量1.0 mL/min,检测波长281 nm,柱温25 ℃,测定冠脉通片中的丹参素。结果 薄层鉴别中样品色谱斑点清晰,分离较好;气相色谱中,冰片中龙脑及内标物水杨酸甲酯均得到良好的分离,冰片的平均回收率为96.72%(RSD为0.67%);HPLC测定丹参素在0.100 8~0.604 8 μg与峰面积值线性关系良好(r=0.999 8),平均回收率为100.22%(RSD为1.15%)。结论 本实验建立的方法简便、准确、可靠,可用于冠脉通片的质量控制。
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[Abstract]
Objective To establish quality standard for Guanmaitong Tablets. Methods Taking methylbenzene-ethyl acetate-formic acid and butyl acetate-formic acid-water as developing agent, Polygoni Multiflori Radix and Epimedii Folium were identified by TLC. The internal standard method was employed. Methyl salicylate, as internal standard, was added to the sample before treatment. The GC system consisted of Agilent DB-WAX, FID as the detector, nitrogen as carrier gas, and column temperature at 140 ℃. Borneol in Guanmaitong Tablets was determined by GC and salvianolic acid A by HPLC. The chromatographic separation was achieved on a Dikma-C18 column with a mobile phase of methanol-0.5% acetic acid solution (88 : 12). The flow rate was 1.0 mL/min; The detection wavelength was set at 281 nm, and column temperature at 25 ℃. Results TLC spots developed were fairly clear and the blank test showed no interference. Camphol borneol and methyl salicylate were separated well under the chromatographic condition. The average recovery of synthetic borneol was 96.72%. The calibration curve was linear within range of 0.100 8—0.604 8 μg (r = 0.999 8). The average recovery was 100.22%. Conclusion The method is accurate, sensitive, and specific. It could be used for the quality control of Guanmaitong Tablets.
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