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目的:建立用高效液相色谱法(HPLC)测量中药吴茱萸中吴茱萸次碱含量的方法。方法:以甲醇为溶剂,进行不同提取方法对吴茱萸次碱提取试验,设计正交试验,考察浸泡时间、提取时间、溶剂用量为3因数,采用L9(34)正交试验表,HPLC法检测。色谱柱:Welchrom-C18(5μm,250 mm×4.6 mm);流动相:乙腈—水(67:33),流速:1.0 ml/min,柱温:22℃,检测波长:290 nm。结果:回流提取法提取效率较高,吴茱萸次碱的最佳提取条件为用100 ml甲醇浸泡30 min回流提取75 min。吴茱萸次碱的回归方程为Y=2×106X-9078.7,相关系数r=0.9999,其线性范围为0.1002~1.1952μg,平均回收率为100.21%,RSD1.47%。吴茱萸中吴茱萸次碱的含量为0.279%。结论:方法稳定、重现性好、操作简单、结果准确,是检测吴茱萸中吴茱萸次碱较理想的方法。
Objective: To establish a method for the determination of rutaecarpine in Evodia rutaecarpa by high performance liquid chromatography (HPLC). Methods: The extraction of rutaecarpine by different extraction methods was studied with methanol as the solvent. The orthogonal experiment was designed. The soaking time, extraction time and the amount of solvent were 3 factors. The L9 (34) orthogonal test table was used to determine the content of rutaecarpine. Column: Welchrom-C18 (5 μm, 250 mm × 4.6 mm); mobile phase: acetonitrile-water (67:33); flow rate: 1.0 ml / min; Results: The extraction efficiency of reflux extraction was high. The optimal extraction condition of rutaecarpine was extracted with 100 ml methanol for 30 min and extracted for 75 min. The regression equation of rutaecarpine was Y = 2 × 106X-9078.7, the correlation coefficient was 0.9999, the linear range was 0.1002-1.1952μg, the average recovery was 100.21% and RSD was 1.47%. The content of rutaecarpine in Evodia was 0.279%. Conclusion: The method is stable, good reproducibility, simple operation and accurate results. It is an ideal method for the determination of rutaecarpine in Evodia rutaecarpa.