目的 建立基于多指標含量測定及特征圖譜的金沙藤Lygodii Herba對照提取物的質(zhì)量控制方法。方法 采用Waterssymmetry shield^TM RP18（250 mm×4.6 mm，5 μm）色譜柱，以乙腈為流動相A、0.4%磷酸為流動相B，梯度洗脫（0～40 min：90%～75% B，40～45 min：75%～60% B，45 ～ 50 min ： 60%～ 10% B ），柱溫30℃，體積流量為1 mL·min^-1，檢測波長為354 nm；測定3批次金沙藤對照提取物中咖啡酸、異槲皮苷、山柰酚-3-O-蕓香糖苷和紫云英苷的含量；建立特征圖譜方法，并對3批次提取物特征峰進行指認；同時考察引濕性和水分含量。結(jié)果 咖啡酸、異槲皮苷、山柰酚-3-O-蕓香糖苷和紫云英苷各化合物在檢測質(zhì)量濃度范圍內(nèi)線性關(guān)系良好（r＞0.999 9），進樣精密度RSD在0.2%～0.3%，重復性RSD在0.4%～0.5%，4種成分的加樣回收率在92.5%～101.0%，樣品溶液中各成分在48 h內(nèi)穩(wěn)定性良好。3批次對照提取物中，咖啡酸質(zhì)量分數(shù)為0.50%～0.64%，異槲皮苷質(zhì)量分數(shù)為0.14%～0.21%，山柰酚-3-O-蕓香糖苷質(zhì)量分數(shù)為0.11%～0.36%，紫云英苷質(zhì)量分數(shù)為0.66%～0.80%。通過建立的提取物HPLC特征圖譜，確定了4個共有特征峰，并根據(jù)對照品對色譜峰進行確認，3批次提取物質(zhì)量差異較小。金沙藤對照提取物水分含量為1.4%～2.3%，具引濕性。結(jié)論 建立的多指標含量測定方法和特征圖譜方法簡便、快速、準確性高、重復性好，可用于金沙藤對照提取物的質(zhì)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

科技部重大新藥創(chuàng)制(2018ZX09303-024,2018ZX09735-006)