HPLC-RID测定银杏达莫注射液中银杏内酯含量

目的: 建立银杏达莫注射液中银杏内酯的快速测定方法。方法: 采用酸性氧化铝柱处理银杏达莫注射液样品代替常用的乙酸乙酯萃取富集内酯的前处理方法,采用HPLC-RID测定银杏达莫注射液中银杏内酯含量。色谱条件:采用大连依力特Hypersil ODS2色谱柱(150 mm×4.6 mm,5 μm),以甲醇-水(28:72)为流动相,流速0.80 mL·min^-1,柱温(35±0.1)℃,以示差折光检测器检测。结果: 白果内酯、银杏内酯A、银杏内酯B和银杏内酯C质量浓度分别在40.80~116.57、47.65~136.28、53.35~152.58、49.80~142.29 μg·mL^-1范围内呈良好的线性关系,回归方程分别为Y=133.66X-655.23(R²=0.992 1)、Y=151.23X-165.51(R²=0.993 3)、Y=184.80X-218.83(R²=0.992 8)、Y=171.94X-537.89 (R²=0.994 6),平均回收率分别为103.4%(RSD=1.11%)、100.1%(RSD=1.85%)、102.7%(RSD=1.47%)、101.1%(RSD=1.69%)。结论: 用酸性氧化铝干柱法处理银杏达莫注射液能有效地去除杂质对内酯测定的干扰,与乙酸乙酯多级萃取处理样品方法相比,减少了样品前处理时间,可用于银杏达莫注射液的银杏内酯的测定,以便控制其质量。

Objective: To establish an HPLC-RID method for the determination of bilobide,ginkgolide A,ginkgolide B and ginkgolide C in ginkgo leaf extract and dipyidamole injection. Methods: The chromatographic process was performed on a Hypersil ODS2 column(150 mm×4.6 mm,5 μm) with the mobile phase of methanol-water(28:72) at a flow rate of 0.8 mL·min^-1.The column temperature was controlled at (35±0.1)℃,and refractive index detector(RID) was used. Results: The linear ranges of bilobide,ginkgolide A,ginkgolide B and ginkgolide C were 40.80-116.57(R²=0.992 1)、47.65-136.28(R²=0.993 3)、53.35-152.58(R²=0.992 8)、and 49.80-142.29(R²=0.994 6) μg·mL^-1,respectively.The average recoveries of bilobide,ginkgolide A,ginkgolide B and ginkgolide C were 103.4%(RSD=1.11%),100.1%(RSD=1.85%),102.7%(RSD=1.47%) and 101.1%(RSD=1.69%),respectively. Conclusion: The established HPLC-RID method was precise,reproducible and stable,which can be applied in the quality control of ginkgo leaf and dipyridamole injection.