论文部分内容阅读
目的 建立银杏酸的反相银化高效液相色谱分离和含量测定方法。方法 用LC ESI MS对银杏叶中银杏酸进行鉴定 ,并用反相银化HPLC研究 4种银杏酸的分离和含量测定。在银杏叶的乙醇浸提液中加入酸性盐溶液和少量吸附剂后 ,用正己烷萃取 ,N2 浓缩后的残留物进行HPLC分析。流动相为甲醇 5 %乙酸 (90∶10 ) ,其中银离子浓度为 0 0 3mol·L- 1 ,HPLC和二极管阵列检测联用对银杏酸色谱峰进行光谱分析和纯度鉴定。结果 反相银化HPLC分析银杏酸所确定的色谱峰是正确的 ,4种银杏酸与杂质成分均完全分离。平均回收率 97 3% ,方法的精密度RSD为 1 6 %。结论 反相银化HPLC是分离碳数与饱和度均不相同的同系物的有效方法 ,可用于银杏酸的定量分析和银杏叶生产的质量控制
Objective To establish a reversed phase silverization high performance liquid chromatography (HPLC) method for the separation and determination of ginkgo acid. Methods Ginkgo biloba was identified in Ginkgo biloba L. by LC ESI MS. The separation and determination of four ginkgo acids were determined by reverse phase silverization HPLC. An acidic salt solution and a small amount of adsorbent were added to the ethanol extract of Ginkgo biloba leaves, extracted with n-hexane, and the residue after N2 concentration was subjected to HPLC analysis. The mobile phase consisted of 5 % acetic acid (90:10) methanol, and the silver ion concentration was 0.03 mol·L -1 , and the chromatographic peaks of ginkgolic acid were analyzed by HPLC and diode array detection. Results The chromatographic peaks determined by reversed-phase silverization HPLC analysis of ginkgolic acid were correct. The four ginkgolic acids and impurities were completely separated. The average recovery rate was 97 3%. The precision of the method RSD was 16%. Conclusion Inverse-phase silverization HPLC is an effective method for separating homologs with different carbon numbers and saturations. It can be used for quantitative analysis of ginkgo acid and quality control of Ginkgo biloba leaf production.