[關(guān)鍵詞]
[摘要]
目的 建立槐枝Sophora japonica HPLC指紋圖譜和多成分含量測(cè)定方法,結(jié)合化學(xué)模式識(shí)別法對(duì)槐枝藥材進(jìn)行質(zhì)量評(píng)價(jià)。方法 采用HPLC法,以甲醇∶乙腈(1∶ 1,A)-0.1%磷酸水溶液(B)為流動(dòng)相梯度洗脫,柱溫40℃,檢測(cè)波長(zhǎng)258 nm,體積流量1.2 mL·min-1。建立15批槐枝藥材的指紋圖譜并分析相似度,測(cè)定其中6種成分(染料木苷、蘆丁、芹菜苷、山柰酚-3-O-蕓香糖苷、水仙苷、染料木素)的含量,結(jié)合聚類(lèi)分析(HCA)、主成分分析(PCA)及正交偏最小二乘法分析(OPLS-DA)進(jìn)行質(zhì)量評(píng)價(jià)。結(jié)果 15批槐枝指紋圖譜共標(biāo)定12個(gè)共有峰,指認(rèn)出染料木苷、蘆丁、芹菜苷、山柰酚-3-O-蕓香糖苷、水仙苷、染料木素6個(gè)成分,各批次相似度在0.780~0.996。建立6個(gè)成分HPLC含量測(cè)定方法,樣品中染料木苷、蘆丁、芹菜苷、山柰酚-3-O-蕓香糖苷、水仙苷、染料木素質(zhì)量分?jǐn)?shù)分別為0.006~0.113、0.378~3.782、0.280~4.397、0.112~0.561、0.036~0.427、0.003~0.047 mg·g-1。HCA結(jié)果將15批槐枝分為3類(lèi); PCA提取了3個(gè)主成分,3個(gè)主成分在反映不同批次槐枝樣品共有成分關(guān)系中起主要作用。OPLS-DA結(jié)果表明,芹菜苷和蘆丁為引起質(zhì)量差異的標(biāo)志性成分。結(jié)論 建立的槐枝HPLC指紋圖譜及多成分含量測(cè)定方法操作簡(jiǎn)便,結(jié)果可靠,為槐枝的質(zhì)量評(píng)價(jià)提供依據(jù)。
[Key word]
[Abstract]
Objective To establish an HPLC fingerprint and a multi-component quantification method for Sophora japonica Linn., and to evaluate the quality of S. japonica medicinal materials using chemical pattern recognition methods. Methods The HPLC method was performed with the gradient elution of methanol-acetonitrile (1∶ 1, A)-0.1% aqueous phosphoric acid (B) as the mobile phase, the column temperature was 40 ℃, the detection wavelength was 258 nm, and the volume flow rate was 1.2 mL·min-1. Fingerprints of 15 batches of S. japonica herbs were established and analysed for similarity, and the contents of six constituents (genistein, rutin, apigenin, kaempferol-3-O-rutinoside, silymarin and genistein) were determined and combined with HCA, PCA and OPLS-DA for quality evaluation. Results The fingerprints of 15 batches of S. japonica were calibrated with 12 common peaks, recognising six components: genistein, rutin, apigenin, kaempferol-3-O-rutinoside, silymarin and genistein, with the similarity of the batches in the range of 0.780~0.996. HPLC methods were established for the determination of the content of these six components, and contents of genistein, rutin, apigenin, kaempferol-3-O-rutinoside, silymarin and genistein in the samples ranged from 0.006 to 0.113, from 0.378 to 3.782, from 0.280 to 4.397, from 0.112 to 0.561, from 0.036 to 0.427, from 0.003 to 0.047 mg·g-1. The results of cluster analysis classified the 15 batches of acacia twigs into three categories; PCA extracted three principal components, indicating that the three principal components played a major role in reflecting the relationship between the common components of acacia twigs samples from different batches. The results of OPLS-DA indicated that apigenin and rutin were the signature components that caused the quality differences. Conclusion The established HPLC fingerprints of S. japonica and the method for the determination of multicomponent content were easy to operate and the results were reliable, which provided the basis for the quality evaluation of S. japonica.
[中圖分類(lèi)號(hào)]
R284.1
[基金項(xiàng)目]
國(guó)家重點(diǎn)研發(fā)計(jì)劃-中醫(yī)藥現(xiàn)代化專(zhuān)項(xiàng)(2023YFC3504101);北京中醫(yī)藥大學(xué)縱向科研發(fā)展基金項(xiàng)目( 2024-ZXFZJJ-JW-010)