Yang Liu-qing, Wu Xiang-yang, Chen Jun
School of Pharmacy, Jiangsu University, Zhenjiang 212013, China.
Yao Xue Xue Bao. 2002 Jul;37(7):555-8.
To establish a simple pre-treated method and high performance liquid chromatographic method for separation and determination of ginkgolic acids in Ginkgo biloba leaves.
The ginkgolic acids in the German standard sample were identified by LC/DAD/ESI/MS. The methods for pre-treatment and high performance liquid chromatography determination of ginkgolic acids were studied. Ginkgo biloba leaves were extracted with n-hexane in Soxhlet apparatus, then concentrated under vacuum. The ginkgolic acids can be determined directly by HPLC after one-pre-purified-step by silica gel column chromatography. The eluant was petroleum ether-diethyl ether-formic acid (89:11:1). The chromatographic column was Inertsil ODS-2; the mobile phase was methanol-3% acetic acid (92:8); the flow rate was 1.0 mL.min-1; the column temperature was 40 degrees C; the detection wavelength was at 310 nm.
There were five kinds of ginkgolic acid (C13:0, C15:1, C17:2, C15:0 and C17:1) in ginkgo biloba leaves. The relative percentage content of ginkgolic acids C15:1 and C17:1 was about 85%. Ginkgolic acid C17:2 had not been reported in China. The HPLC indicates that there was nearly no impurities except ginkgolic acids after treated by column chromatography. The results showed that the content of ginkgolic acids in the leaves of Ginkgo biloba collected in April, May and June was 1.48%, 1.19% and 1.11% respectively. The average recovery of Ginkgo biloba leaves collected in June was 97.0%, RSD was 1.7% (n = 6).
The method is accurate, simple and reliable, and can be used for determination of ginkgolic acids in Ginkgo biloba leaves.
建立一种简单的预处理方法和高效液相色谱法，用于分离和测定银杏叶中的银杏酸。
采用液相色谱-二极管阵列检测器-电喷雾电离质谱联用（LC/DAD/ESI/MS）对德国标准样品中的银杏酸进行鉴定。研究了银杏酸的预处理方法和高效液相色谱测定方法。银杏叶用正己烷在索氏提取器中提取，然后减压浓缩。经硅胶柱色谱一步预纯化后，可直接用高效液相色谱法测定银杏酸。洗脱剂为石油醚-乙醚-甲酸（89:11:1）。色谱柱为Inertsil ODS-2；流动相为甲醇-3%乙酸（92:8）；流速为1.0 mL·min-1；柱温为40℃；检测波长为310 nm。
银杏叶中含有5种银杏酸（C13:0、C15:1、C17:2、C15:0和C17:1）。银杏酸C15:1和C17:1的相对百分含量约为85%。银杏酸C17:2在国内未见报道。高效液相色谱分析表明，柱色谱处理后除银杏酸外几乎无杂质。结果表明，4月、5月和6月采集的银杏叶中银杏酸的含量分别为1.48%、1.19%和1.11%。6月采集的银杏叶平均回收率为97.0%，相对标准偏差为1.7%（n = 6）。
该方法准确、简便、可靠，可用于银杏叶中银杏酸的测定。
