银杏叶中莽草酸含量高效液相色谱测定方法研究

Determination of shikimic acid in ginkgo biloba leaves by HPLC

本研究建立了高效液相色谱法测定银杏叶中莽草酸含量的方法。称取银杏叶样品粉末1.0 g,用0.1%磷酸水定容至100 mL,提取功率320 W,提取时间70 min,提取温度55℃,采用HPLC进行测定。建立的液相条件为:以乙腈:0.1%磷酸水作为流动相,以C18色谱柱为固定相,进行梯度洗脱,流速为0.8 mL/min,检测波长210 nm。结果显示,质量浓度在0.0072~0.4598 mg/mL范围内与其对应的峰面积呈线性关系(R^(2)>0.9999),检出限(3S/N)为0.07 mg/mL,日内(n=6)和日间(n=9)测定值的相对标准偏差(RSD)分别为0.95%和0.90%;对银杏叶样品进行3个浓度水平的回收试验,莽草酸含量的回收率在95.75%~102.25%之间,满足GB27404-2008《试验室质量控制规范食品理化检测》中的回收率要求。该方法稳定性好、准确性高,且操作简单、快速,可用于大批量分析测定银杏叶中莽草酸含量,具有较高实用价值。

A HPLC method for the determination of shikimic acid in ginkgo biloba leaves was established.The powder of ginkgo biloba leaves was measured by HPLC with 1.0 g of the sample,and was filled to 100 mL with 0.1% phosphoric acid water.The extraction power was 320 W,extraction time was 70 min and extraction temperature was 55℃.The established liquid phase conditions were as follows:acetonitrile:0.1% phosphoric acid water as mobile phase,C18 column as stationary phase,gradient elution,flow rate of 0.8 mL/min,and detection wavelength 210 nm.The results showed that there was a linear relationship between the mass concentration and the corresponding peak area in the range of 0.0072〜0.4598 mg/mL(R^(2)>0.9999),and the detection limit(3S/N)was 0.07 mg/mL.The relative standard deviations(RSD)of intra-day(n=6)and intra-day(n=9)measurements were 0.95% and 0.90%,respectively.Three concentration levels of ginkgo biloba samples were recovered,and the recovery rate of shikimic acid was between 95.75%〜102.25%,which was in line with the recovery rate requirements of GB27404-2008《Laboratory Quality Control Standard Physicochemical Testing of food》.The method is stable,accurate,simple and rapid,and can be used for the determination of shikimic acid in Ginkgo biloba leaves.