18色譜柱(250 mm×4.6 mm,5 μm);流動(dòng)相:甲醇-10 mmol乙酸銨水溶液,梯度洗脫;柱溫:30℃;體積流量:1 mL/min;進(jìn)樣量:10 μL。采用離子阱(ESI)負(fù)離子模式進(jìn)行檢測(cè),檢測(cè)模式為母離子全掃描方式(Scan),并進(jìn)行二次離子化掃描。霧化器壓力310.28 kPa,毛細(xì)管電壓3.5 kV,碰撞誘導(dǎo)解離電壓150 V,干燥氣為N2,干燥器溫度350℃,干燥氣流量8.0 L/min。結(jié)果 銀杏內(nèi)酯A、B、C和白果內(nèi)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/mL顯示良好的線(xiàn)性關(guān)系;平均加樣回收率分別為97.1%、97.0%、98.2%、97.8%,RSD值分別為1.73%、1.68%、1.76%、1.83%(n=6)。結(jié)論 該法靈敏度高、選擇性高、檢測(cè)限低,為銀杏葉片的質(zhì)量控制提供依據(jù)。;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-C18 column (250 mm×4.6 mm, 5 μm). 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 5 μL. 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. Results There were good linear relationships of ginkgolide A, ginkgolide B, ginkgolide C, and bilobalide in the concentration ranges of 0.100 6-2.012 0, 0.102 0-2.040 0, 0.050 0-1.000 0, and 0.101 6-2.032 0 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."/>