高效液相色谱法测定银杏叶提取物及其制剂中银杏酸的含量

Determination of ginkgolic acids in Ginkgo biloba extract and its preparations by high performance liquid chromatography

目的 建立银杏叶提取物及其制剂中银杏酸含量的HPLC测定方法。方法 银杏叶提取物及其制剂经石油醚提取 ,提取液浓缩后用石油醚定容 ,HPLC直接测定 ,并用LC MS对其中的银杏酸进行了定性鉴定。色谱分析条件 :色谱柱为InertsilODS 2 ,流动相为甲醇 3%HAc溶液 (92∶8) ,流速 1 0mL·min- 1 ,柱温 4 0℃ ,紫外检测波长310nm。结果 银杏叶提取物中存在 6种银杏酸C13:0 ,C15 :0 ,C15 :1,C17:1,C17:2和一种可能是C17∶3的银杏酸化合物 ,其中C13∶0 ,C15∶1和C17∶1占总银杏酸的 94 %以上。实验测得高银杏酸含量的提取物中银杏酸含量为1 12 % ,RSD为 2 4 % (n =5 ) ;银杏叶提取物片剂中银杏酸含量为 4 9 2 μg·g- 1 ,RSD为 4 3% (n =5 )。平均回收率98 2 % ,RSD为 2 6 % (n =5 )。结论 该方法准确、快速、简便 。

Aim To establish a high performance liquid chromatographic method for determination of ginkgolic acids in Ginkgo biloba extract and its preparations. Methods Ginkgo biloba extract and its preparations were extracted with petroleum ether in Soxhlet apparatus, and then concentrated under vacuum. The ginkgolic acids were determined directly by HPLC, and identified by LC/DAD/ESI/MS. The chromatographic column was Inertsil ODS-2; the mobile phase was methanol-3% aqueous acetic acid(92∶8); the flow rate was 1...