目的 建立基于多指标含量测定及特征图谱的金沙藤Lygodii Herba对照提取物的质量控制方法。方法 采用Waterssymmetry shield^TM RP18（250 mm×4.6 mm，5 μm）色谱柱，以乙腈为流动相A、0.4%磷酸为流动相B，梯度洗脱（0～40 min：90%～75% B，40～45 min：75%～60% B，45 ～ 50 min ： 60%～ 10% B ），柱温30℃，体积流量为1 mL·min^-1，检测波长为354 nm；测定3批次金沙藤对照提取物中咖啡酸、异槲皮苷、山柰酚-3-O-芸香糖苷和紫云英苷的含量；建立特征图谱方法，并对3批次提取物特征峰进行指认；同时考察引湿性和水分含量。结果 咖啡酸、异槲皮苷、山柰酚-3-O-芸香糖苷和紫云英苷各化合物在检测质量浓度范围内线性关系良好（r＞0.999 9），进样精密度RSD在0.2%～0.3%，重复性RSD在0.4%～0.5%，4种成分的加样回收率在92.5%～101.0%，样品溶液中各成分在48 h内稳定性良好。3批次对照提取物中，咖啡酸质量分数为0.50%～0.64%，异槲皮苷质量分数为0.14%～0.21%，山柰酚-3-O-芸香糖苷质量分数为0.11%～0.36%，紫云英苷质量分数为0.66%～0.80%。通过建立的提取物HPLC特征图谱，确定了4个共有特征峰，并根据对照品对色谱峰进行确认，3批次提取物质量差异较小。金沙藤对照提取物水分含量为1.4%～2.3%，具引湿性。结论 建立的多指标含量测定方法和特征图谱方法简便、快速、准确性高、重复性好，可用于金沙藤对照提取物的质量控制。

Objective To determine the multi-index content of the reference extract of Lygodii Herba and the quality control method of characteristic spectrum. Method Waters symmetry shield^TM RP18 (250 mm×4.6 mm, 5 μm) column was used. Using acetonitrile as mobile phase A, 0.4% phosphoric acid as mobile phase B, gradient elution (0—40 min: 90%—75% B, 40—45 min: 75%—60% B, 45—50 min: 60%—10% B), column temperature 30 ℃, flow rate 1 mL·min^-1, detection wavelength 354 nm. Determined the content of caffeic acid, isoquercitrin, kaempferol-3-O-rutinoside and astragaloside in three batches of Lygodii Herba control extracts. Moreover, a characteristic map method was established and the characteristic peaks of the three batches of extracts were identified. Simultaneously examine moisture absorption and moisture. Results Caffeic acid, isoquercitrin, kaempferol-3-O-rutinoside and astragaloside had a good linear relationship in the respective detection mass concentration ranges (r>0.999 9), and the injection precision RSD was 0.2%—0.3%, the reproducible RSD was 0.4%—0.5%, and the recovery of the six components was 92.5%— 101.0%. The stability of each component in the sample solution was good within 48 h. In the three batches of control extracts, the content of caffeic acid was between 0.50% and 0.64%, the content of isoquercitrin was between 0.14% and 0.21%, and the content of kaempferol-3-O-rutinoside was between 0.11% and 0.36%, the content of astragalus glycosides was between 0.66% and 0.80%. Through the established HPLC characteristic spectrum of the extract, four common characteristic peaks were determined, and the chromatographic peaks were confirmed according to the reference substance. The quality difference of the three batches of extracts was small. The moisture content of the control extract of Lygodii Herba was between 1.4%—2.3%, which was hygroscopic. Conclusion The multi-index content determination method and fingerprint method established in this study were simple, rapid, accurate and reproducible, and can be used for quality control of Lygodii Herba control extract.

R286.02

科技部重大新药创制(2018ZX09303-024,2018ZX09735-006)