鸡血藤药材中原儿茶酸的含量测定

建立测定鸡血藤药材中原儿茶酸含量的方法,并对制备供试品溶液的提取溶剂、提取方法、提取次数、药材粒度等进行了考察优化。采用高效液相色谱法,色谱柱:Diamonsil C18色谱柱(250×4.6 mm,5μm);流动相为乙腈-φ=0.5%醋酸水(体积比为10∶90);流速为1.0 mL·min-1;检测波长为260 nm。优化所得供试品溶液的制备方法,药材加水回流提取3次,每次1.5 h,合并提取液并浓缩至小体积,用乙酸乙酯萃取4次,合并乙酸乙酯萃取液,浓缩后的残渣用甲醇-水(体积比为1∶1)溶解并定容,即得。经系统的方法学考察,所建立的方法在原儿茶酸浓度为8.56~214μg·mL-1范围内线性良好(R2=0.999 7),平均加样回收率为99.2%,RSD为2.8%,市售7个批次鸡血藤药材中原儿茶酸的含量为65.81~122.35μg·g-1。该方法准确,重复性好,可用于鸡血藤药材的质量控制。

Determination of Protocatechuic Acid in Spatholobi Caulis

High performance liquid chromatography (HPLC) was developed for the quantitative analysis of protocatechuic acid (PA) in Spatholobi Caulis (the stem of Suberect spatholobus Dunn.). The preparation method of sample solution was established by optimizing the extraction solvents, methods, times and the sizes of the crude drug. The sample solutions were analyzed using a C₁₈ column ( 250 × 4.6 mm，5μm) with CH3CN-φ=0.5% HAc (volumic ratio,10:90) as mobile phase and detected at 260 nm with a flow rate of 1.0 mL·min^-1. The crude drug was extracted by boiling water for three times and 1.5 h for each time. The obtained aqueous solution was concentrated and followed by extracted with ethyl acetate for four times. The ethyl acetate layer was concentrated to dryness, and was resolved in methanol-water (volumic ratio,1:1) to give the sample solution previous to HPLC analysis. After systematic method evaluation, the results showed that the linear range was 8.56～214 μg·mL^-1 with correlation coefficient R² of 0.999 7; and the average recovery rate was 99.2% with RSD of 2.8%. The contents of PA in market sold seven batches of Spatholobi Caulis were determined to be in the range of 65.81～122.35 μg·g^-1. The established method was accurate and repeatable, which could be used for the quality control of Spatholobi Caulis.