目的 建立银杏二萜内酯提取物中大分子物质的高效液相体积排阻色谱(HPSEC-RI)检测方法。方法 色谱柱为Phenomenex Biosep-SEC-S2000(300 mm×7.8 mm,5 μm);以0.05 mol/L硫酸钠为流动相;体积流量为0.7 mL/min;柱温30 ℃;示差检测器,按面积归一化法计算大分子物质的质量分数。结果 相对分子质量在2 500～84 400的物质,其相对分子质量对数-保留时间呈现良好的线性关系(r=0.998 3);平均回收率为96.8%,RSD为1.5%;5批银杏二萜内酯提取物和14批银杏二萜内酯葡胺注射液均未检出大分子物质。结论 本方法简便易行,结果准确可靠,可作为银杏二萜内酯提取物及银杏二萜内酯葡胺注射液质量控制方法。

Objective To establish a high performance size exclusion chromatography (HPSEC) method for the determination of high molecular weight substances in ginkgo diterpene lactone extraction. Methods The chromatographic column Phenomenex Biosep-SEC-S2000 (300 mm × 7.8 mm, 5 μm) was used with 0.05 mol/L sodium sulfate as the mobile phase at a flow rate of 0.7 mL/min, with refractive index detector (RID), and the temperature of the column was 30 ℃. High molecular weight substances in samples were calculated with area normalization method. Results In the range of 2 500—84 400 of substance molecular weights, a linearity was achieved (r = 0.998 3). The average recovery rate was 96.8%, and RSD was 1.5%. The high molecular weight substances in five batches of ginkgo diterpene lactone extraction were not detected. Conclusion This method is simple, quick, accurate, and suitable for the quality control of high molecular weight substances in ginkgo diterpene lactone extraction.

科技部重大新药创制：现在中药创新集群与数字制药科技平台(2013ZX09402203);国家重大科技成果转化专项