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机构地区:[1]湖北中医药大学,湖北武汉430065 [2]湖北省随州市食品药品监督检验所,湖北随州441300
出 处:《湖北中医药大学学报》2013年第3期38-41,共4页Journal of Hubei University of Chinese Medicine
摘 要:目的建立高效液相色谱(HPLC)法同时测定清开灵颗粒中绿原酸和黄芩苷含量分析方法。方法用C18硅胶柱(150mm×4.6mm,5μm)为固定相,甲醇-0.4%的磷酸水溶液为流动相,进行梯度洗脱,流速为1mL/min,紫外检测波长为323nm。结果绿原酸和黄芩苷的线性范围分别为5.567-139.4μg/mL和8.640-216.0μg/mL;相关系数分别为0.9995和0.9997;加样平均回收率分别为99.77%和100.68%;检出限分别为0.05μg和0.06μg;精密度实验RSD分别为0.99%、1.45%;重现性试验RSD分别为1.48%、0.72%;稳定性试验RSD分别为2.53%、1.45%。4批样品中绿原酸的含量在0.722-1.086 mg/袋,黄芩苷的含量在22.636-23.463 mg/袋。结论该方法简便,快速,准确,灵敏度高,重现性好,成本低,可用于清开灵颗粒的质量控制。Objectve To develop an RP - HPLC method for the determination of chlorogenic acid and baicalin in Qingkailing Granule. Methods A C18(150mm ×4.6mm,5μm) bond silica for reersed -phase HPLC was prepared. The mobile phase was CH3OH -0. 4% Phosphoric acid. The flow rate was set at 1.0ml/min. The detection wavelength was at 323 nm. Chlorogenic acid and baicalin were separated by HPLC with grade elution. Results The linearity ranges of chlorogenic acid and baicalin were 5. 567- 139.4μg,/mL and 8. 640 - 216. 0μg/mL respectively;The correlation coefficient were 0.9995 and 0. 9997;The recoveries of adding sample rate were 99.77% and 100. 68% ;The detection limits were 0.05μg and 0. 06μg. The RSD (n =5) of measurement precisions test were 0.99% and 1.45% ;The RSD ( n = 5) of reproducibility between tests were 1.48% and 0. 72% . The RSD (n = 5 ) of stability test were 2. 53% and 1.45%. The content of chlorogenie acid in compound Qingkailing granule was 0. 722 - 1. 086 mg/bag, and that of baicalin was 22. 636 - 23. 463 mg/bag. Conclusion The method is simple, fast, accurate, sensitive, reproducible and low cost. It is fit for the quality control of compound Qing- kailing Granule.
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