[關(guān)鍵詞]
[摘要]
目的 建立槲寄生黃酮類成分的特征指紋圖譜,同時(shí)測定槲寄生中高圣草素-7-O-β-D-葡萄糖苷、高圣草素的含量,結(jié)合化學(xué)計(jì)量法分析,為其質(zhì)量控制提供參考。方法 采用Agilent ZORBAX SB-C18色譜柱(250 mm×4.6 mm,5 μm),以乙腈-0.1%磷酸溶液為流動(dòng)相,梯度洗脫,體積流量1.0 mL·min-1,檢測波長為285 nm,柱溫30℃。建立14批槲寄生藥材的黃酮類成分指紋圖譜,結(jié)合化學(xué)計(jì)量學(xué)軟件進(jìn)行聚類分析(CA)、主成分分析(PCA)、偏最小二乘法-判別分析(PLS-DA)。在同一色譜條件下,經(jīng)方法學(xué)驗(yàn)證,HPLC法同時(shí)測定14批槲寄生藥材中高圣草素-7-O-β-D-葡萄糖苷、高圣草素。結(jié)果 建立了槲寄生藥材黃酮類成分的指紋圖譜,標(biāo)定了7個(gè)共有特征峰,指認(rèn)了其中2個(gè)峰:峰4 (高圣草素-7-O-β-D-葡萄糖苷)、峰6(高圣草素);其中12批槲寄生藥材相似度達(dá)到0.9以上,聚類分析將14批樣品分為2類;PCA分析共得到2個(gè)主成分,主成分1主要反映了特征峰2~7的信息,主成分2主要反映特征峰1的信息,峰4與峰6的峰面積較大,且對第1主成分的貢獻(xiàn)也較大;PLS-DA結(jié)果表明,3個(gè)共有特征峰的變量重要性投影(VIP)值>1,依次為峰7、峰6、峰4。高圣草素-7-O-β-D-葡萄糖苷、高圣草素2個(gè)指標(biāo)成分在一定質(zhì)量濃度范圍內(nèi)線性關(guān)系良好,平均加樣回收率分別為103.17%、101.47%,RSD分別為2.0%、0.7%,方法學(xué)考察結(jié)果均符合相關(guān)要求,14批樣品中2種成分總質(zhì)量分?jǐn)?shù)為2.32~5.17 mg·g-1。結(jié)論 建立的方法準(zhǔn)確、簡便、重現(xiàn)性好,可為槲寄生藥材的質(zhì)量控制提供參考。
[Key word]
[Abstract]
Objective Under the same chromatographic conditions, establish a characteristic fingerprint of flavonoids in Viscum coloratum, and simultaneously determine the content of homoeriodictyol-7-O-β-D-glycoside and homoeriodictyol, combined with stoichiometric analysis, provides a reference for their quality control. Methods The separation was performed on a ZORBAX SB-C18 column (250 mm×4.6 mm, 5 μm) using a gradient elution with acetonitrile-0.1% phosphoric acid aqueous solution,and the flow rate at 1.0 mL·min-1,the detection wavelength at 285 nm,the column temperature was set at 30 ℃. The flavonoids fingerprints of 14 batches of Viscum coloratum were established, and cluster analysis (CA), principal component analysis (PCA), partial least squares discriminant analysis (PLS-DA) were performed with chemometrics software. Under the same chromatographic conditions, after being validated by formula, HPLC method was used to simultaneously determine the content of homoeriodictyol-7-O-β-D-glycoside and homoeriodictyol. Results The fingerprint of flavonoids in Viscum coloratum was established, seven common peaks were demarcated, and two of them were identified. The similarity of 12 batches of mistletoe was all above 0.9. Cluster analysis divided the 14 batches of samples into two categories. PCA analysis obtained a total of two principal components. Principal component 1 mainly reflects the information of feature peaks 2—7, while principal component 2 mainly reflects the information of feature peak 1. The peak areas of peaks 4 and 6 were larger, and their contribution to the first principal component were also significant. The PLSDA results indicate that the variable importance projection (VIP) values of the three common characteristic peaks are greater than 1, followed by peak 7, peak 6, and peak 4. The content derermination results showed that the two index components of homoeriodictyol-7-O-β-D-glycoside and homoeriodictyol had good linear relationship within a certain mass concentration range.The average recoveries were 103.17% and 101.47%, and the RSDs were 2.0% and 0.7% respectively. The results of content determination Methods met the relevant requirements, and the total content of two components in 14 batches of samples was 2.32— 5.17 mg·g-1. Conclusion The established method was accurate,simple and reproducible,which can provides an exprimental basis for the overall evaluation and quality control of Viscum coloratum.
[中圖分類號]
R284.1
[基金項(xiàng)目]
寒地道地藥材質(zhì)量評價(jià)與開發(fā)利用關(guān)鍵技術(shù)研究及示范項(xiàng)目(GZ20210092)