Krzek Jan, Czekaj Janusz S, Rzeszutko Włodzimierz, Ekiert Radosław J
Department of Inorganic and Analytical Chemistry, Collegium Medicum, Jagiellonian University, 9 Medyczna St., 30-688 Kraków, Poland.
Acta Pol Pharm. 2007 Jul-Aug;64(4):303-10.
A method for identification and quantitative determination of ginkgolides A, B, and C and bilobalide in liquid and dry extracts of Ginkgo biloba extracts has been developed. Determinations made by employing capillary gas chromatography technique with FID detection were preceded by derivatization using BSTFA with TMCS addition at 120 degrees C. Cholesterol was used as an internal standard. Validation of the method shows no interferences with concurrent constituents; average resolution (R), controlled for peaks of cholesterol and ginkgolide A was 1.53 (SD = 0.06). In the temperature program used (from 50 degrees C to 300 degrees C) the analyte retention times range from 11.2 min. (bilobalide) to 13.8 min. (ginkgolide C) and are of high repeatability of relative values (RRT): RSD = 0.05% / 0.07% for ginkgolides. High correlation coefficients (r), detector signal linearity: from 0.99962 for ginkgolide C to 0.99985 for ginkgolide A were obtained within the concentration range under investigation. The method is of high sensitivity: limits of detection and limits of determination are 35 pg and 44 pg for bilobalide, respectively, while for ginkgolides (Gk) are: 78 pg and 92 pg for GkA, 57 pg and 68 pg for GkB, and 213 pg and 320 pg for GkC.
已开发出一种用于鉴定和定量测定银杏叶提取物的液体和干提取物中银杏内酯A、B、C和白果内酯的方法。采用带氢火焰离子化检测器（FID）的毛细管气相色谱技术进行测定之前，需在120℃下使用含三甲基氯硅烷（TMCS）的N,O-双（三甲基硅基）三氟乙酰胺（BSTFA）进行衍生化。使用胆固醇作为内标。该方法的验证表明，其不受共存成分的干扰；针对胆固醇和银杏内酯A的峰，平均分离度（R）为1.53（标准差=0.06）。在所使用的温度程序（从50℃至300℃）中，分析物的保留时间范围为11.2分钟（白果内酯）至13.8分钟（银杏内酯C），且相对值具有高重复性（相对保留时间：RRT）：银杏内酯的相对标准偏差（RSD）=0.05%/0.07%。获得了高相关系数（r），检测器信号线性：在所研究的浓度范围内，银杏内酯C的相关系数为0.99962，银杏内酯A的相关系数为0.99985。该方法具有高灵敏度：白果内酯的检测限和定量限分别为35皮克和44皮克，而银杏内酯的检测限和定量限分别为：银杏内酯A为78皮克和92皮克，银杏内酯B为57皮克和68皮克，银杏内酯C为213皮克和320皮克。
