HPLC-MS法测定银杏叶片中银杏内酯A、B、C和白果内酯

目的建立测定银杏叶片中银杏内酯A、B、C及白果内酯的HPLC-MS法。方法采用HPLC-MS法,Zorbax SB-C_(18)色谱柱(250 mm×4.6 mm,5μm);流动相:甲醇–10 mmol乙酸铵水溶液,梯度洗脱;柱温:30℃;体积流量:1 m L/min;进样量:10μL。采用离子阱(ESI)负离子模式进行检测,检测模式为母离子全扫描方式(Scan),并进行二次离子化扫描。雾化器压力310.28 k Pa,毛细管电压3.5 k V,碰撞诱导解离电压150 V,干燥气为N_2,干燥器温度350℃,干燥气流量8.0 L/min。结果银杏内酯A、B、C和白果内酯在0.100 6~2.012 0、0.102 0~2.040 0、0.050 0~1.000 0、0.101 6~2.032 0 mg/m L显示良好的线性关系;平均加样回收率分别为97.1%、97.0%、98.2%、97.8%,RSD值分别为1.73%、1.68%、1.76%、1.83%(n=6)。结论该法灵敏度高、选择性高、检测限低,为银杏叶片的质量控制提供依据。

Determination of ginkgolid A, B, and C, and bilobalide from Yinxingye Tablets by HPLC-MS method

Objective To establish determination of ginkgolide A, ginkgolide B, ginkgolide C, and bilobalide in Yinxingye Tablets by HPLC-MS.Methods HPLC-MS method was adopted. The determination was carried out on Zorbax SB-C18column (250 mm × 4.6 mm, 5μm). consisted of methanol - 10 mmol ammonium acetate aqueous solution with gradient elution. The column temperature was set at 30℃ at a flow rate of 1.0 mL/min. Injection volume was 5μL. The ion trap (ESI) negative ion mode was used as detection mode, the detection mode was the full scan mode (Scan) of the parent ion, and the two ionization scan was performed. Atomizer pressure was set at 310.28 kPa with capillary voltage of 3.5 kV. Fragmentor voltage was selected at 150 V, and dry gas was N2. The dryer temperature and dry gas flow were 350℃ and 8 L/min.ResultsThere were good linear relationships of ginkgolide A, ginkgolide B, ginkgolide C, and bilobalide in the concentration ranges of 0.1006 — 2.0120, 0.1020 —2.0400, 0.0500 —1.0000, and 0.1016 —2.0320 mg/mL, respectively. The average recoveries were 97.1%, 97.0%, 98.2%, and 97.8% with RSD 1.73%, 1.68%, 1.76%, and 1.83%, respectively.Conclusion The method has high sensitivity, high selectivity, and low detection limit which can be used in quantity control for Yinxingye Tablets.