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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,5μm),以甲醇-水(28∶72)为流动相,流速0.80 m L·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、49.80~142.29μg·m L-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 a rapid method for the determination of ginkgolide in Yinxingdamo injection. Methods: The acidic aluminum oxide column was used to treat the ginkgo-damo injection instead of the commonly used ethyl acetate for the extraction of lactone. The HPLC-RID was used to determine the content of ginkgolide in Yinxingdamo injection. The chromatographic conditions were as follows: using a Hypersil ODS2 column (150 mm × 4.6 mm, 5 μm) with methanol-water (28:72) as the mobile phase at a flow rate of 0.80 m L · min- ) ℃, with the refractive index detector detection. Results: The concentrations of bilobalide, ginkgolide A, ginkgolide B and ginkgolide C were good in the range of 40.80-116.57,47.65-136.28,53.35-152.58,49.80-142.29 μg · m L-1, respectively The linear regression equation was 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 The average recoveries 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 treatment of ginkgo-damo injection with acidic alumina dry column can effectively remove the interference of impurity on the determination of lactone. Compared with the method of multi-stage extraction with ethyl acetate, the time of sample preparation can be reduced, Gamo lactone injection of ginkgolide determination, in order to control its quality.