目的 建立千斤拔Moghania RadixHPLC指紋圖譜及多成分定量方法，為其質(zhì)量控制提供參考。方法 采用XBridge^®C₁₈色譜柱（250mm×4.6mm，5μm）為固定相，以乙腈-0.1%乙酸溶液為流動相進行梯度洗脫，體積流量1.0mL·min-1，檢測波長260nm，柱溫30℃；對24批千斤拔（編號為S1～S24，其中S2～S9為采集的新鮮全株植物，實驗室低溫干燥而得，其余樣品為市場購買藥材或飲片）構(gòu)建指紋圖譜，同時測定相關(guān)成分的含量，并結(jié)合聚類分析、主成分分析及正交偏最小二乘法進行全面評價。結(jié)果 24批不同來源千斤拔指紋圖譜共標(biāo)定11個共有峰，指認(rèn)出染料木苷、6″-O-丙二酰基染料木苷、染料木素。相似度計算結(jié)果表明，各批次相似度在0.707～0.981；聚類分析將24批千斤拔分為2類，S2～S5、S6、S8、S9號樣品（均為新鮮全株植物）聚為一類，其他17份樣品聚為一類；經(jīng)主成分分析，主成分1～4是影響樣品質(zhì)量評價的主要因子，選取前4個主因子對不同產(chǎn)地的千斤拔進行評分，24批樣品的綜合得分在5.34～-3.61，說明各批次質(zhì)量差異相對較大；樣品中綜合得分最高是S4，各飲片樣品的綜合得分較低。24批樣品中染料木苷、6″-O-丙二?；玖夏拒?、染料木素質(zhì)量分?jǐn)?shù)分別為0.10～0.57、0.11～2.85、0.15～0.71mg·g^-1，不同批次之間3個成分質(zhì)量分?jǐn)?shù)差異較大，批次之間3個成分含量總體呈現(xiàn)出二低一高的趨勢，建議使用3個成分總和作為質(zhì)量控制指標(biāo)。結(jié)論 建立的HPLC指紋圖譜及多成分含量測定方法穩(wěn)定、可靠，可為千斤拔的質(zhì)量評價提供依據(jù)。

Objective To establish the HPLC fingerprint and muti-component analysis of Moghaniae Radix and provide reference for quality control.Methods Waters XBridge^® C₁₈ column (250 mm×4.6 mm, 5 μm) were performed on HPLC analysis. The mobile phase was acetonitrile (A)-0.1% acetic acid (B) for gradient elution. The flow rate was 1.0 mL·min^-1, the wavelength was 260 nm and the column temperature was 30 ℃. The content and fingerprint of relative ingredients of 24 batches (the numbers were S1-S24, in which S2-S9 were fresh whole plants collected and dried at low temperature in the laboratory, and the other samples were medicinal materials or decoction pieces purchased from the market) were measured simultaneously, combined with cluster analysis, principal component analysis and orthogonal partial least squares-discriminant analysis (OPLS-DA), which were applied in comprehensive analysis.Results The similarity calculation results showed that the similarity of each batch was between 0.707-0.981, and 11 common peaks were calibrated, genistin, 6"-O-malonyl genistein, genistein were identified. Cluster analysis classified the 24 batches of medicinal materials into two categories, samples S2, S3, S4, S5, S6, S8, S9 (all fresh whole plants) were grouped into one group, and the other 17 samples were grouped into one group. According to the principal component analysis, principal component 1-4 was the main factor affecting the quality evaluation of the samples. The first four principal factors were selected to score the samples from different producing areas, and the comprehensive score of 24 batches of samples was between 5.34 and -3.61, indicating that the quality of each batch was relatively different. The highest composite score of the samples was S4, while the composite score of each piece was lower. The quality fractions of genistein, 6"-O-malondiacylgenistein and genistein in 24 batches of samples ranged from 0.10-0.57 mg·g^-1, 0.11-2.85 mg·g^-1 and 0.15-0.71 mg·g^-1, respectively. The quality fractions of the three batches varied greatly among different batches. The contents of the three items in batches generally show a trend of two low and one high. It was suggested to use the sum of the three items as the quality control index.Conclusion The established HPLC fingerprint and multi-component content determination method are stable and reliable, which can provide a reference for the quality evaluation Moghaniae Radix.

R284.1

國家重點研發(fā)計劃(2019YFC1712304);國家自然科學(xué)基金資助項目(81860711);廣西科技基地和人才專項(桂科AD19245124)