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作 者:杨瑞芬[1] 彭家钢[1] 周蓉[1] 达世禄[2] 杨志[3]
机构地区:[1]湖北中医学院,湖北武汉430065 [2]武汉大学化学与分子科学学院,湖北武汉430072 [3]华中科技大学同济医学院,湖北武汉430030
出 处:《时珍国医国药》2007年第1期124-126,共3页Lishizhen Medicine and Materia Medica Research
摘 要:目的建立高效液相色谱(HPLC)法同时测定双黄连粉针剂中绿原酸和黄芩苷外标定量测定方法。方法用自制C8~C13混合型烷基键合硅胶柱(5μm,4.6mm×150mm)为固定相,甲醇和水溶液(用磷酸调pH2.7)为流动相,在C8-C13柱上梯度洗脱,流速为1ml·min^-1,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4.0-100.0mg·ml^-1和8.6—215.0mg·ml^-;相关系数分别为0.99989和0.99997;加样回收率分别为100.53%和99.94%;检测限分别为0.014mg·ml^-1和0.020mg·ml^-1;精密度实验RSD分别为1.12%和0.61%;重现性实验RSD分别为1.14%和0.73%,稳定性实验RSD分别为0.89%和0.54%;4批样品中绿原酸的含量在1.577~1.753mg·ml^-1,黄芩苷的含量在26.02-28.68mg·ml^-1。结论该方法简便,快速,准确,灵敏虚离。重现性好,成本低,可用于双黄连粉针剂的质量控制。Objective To develop an RP - HPLC method for the determination of chlorogenic acid and baicalin in Shuanghuanglian powder injection. Methods A C8- C13 mixedalkyl (51μm,4.6 mm × 150 mm) bond silica for reversed - phase HPLC was prepared. The mobile phase was CH3OH - phosphoric acid solution ( pH 2.7). The flow rate was set at 1. 0 ml/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 4.0 - 100.0 mg/ml and 8.6 - 215.0 mg/ml respectively, the correlation coefficients were 0.999 89 and 0.999 97 ,the average recoveries of adding sample were 100.53% and 99.94%, detection limits were 0. 014 mg/ml and 0. 020 mg/ml, the RSD (n = 5) of measurement precision test were 1. 12% and 0.61%, the RSD ( n = 5) of reproducibility between tests were 0.89% and 0.54%. The content of chlorogenic acid in Shuanghuanglian powder was 1. 577 - 1. 753 mg/ml,and that of baicalin was 26.02 - 28.68 mg/ml. Conclusion The method is simple, fast, accurate,sensitive, reproducible and low cost. It is fit for the quality control of Shuanghuanglian powder.
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