[關(guān)鍵詞]
[摘要]
目的 建立經(jīng)典名方薏苡附子敗醬散(Yiyi Fuzi Baijiang Powder,YFBP)基準(zhǔn)樣品的HPLC指紋圖譜,對(duì)其指標(biāo)性成分(原兒茶酸、綠原酸、咖啡酸、異綠原酸A、異綠原酸C、苯甲酰新烏頭原堿、亞油酸)進(jìn)行定量測(cè)定,研究YFBP的量值傳遞規(guī)律,并結(jié)合化學(xué)模式識(shí)別評(píng)價(jià)其質(zhì)量。方法 通過建立15批YFBP基準(zhǔn)樣品的HPLC指紋圖譜,明確其特征峰歸屬及出膏率范圍,并對(duì)指標(biāo)性成分進(jìn)行定量測(cè)定。同時(shí)采用層次聚類分析(hierarchical cluster analysis,HCA)、主成分分析(principal component analysis,PCA)與正交偏最小二乘法-判別分析(orthogonal partial least squares-discriminant analysis,OPLS-DA),尋找影響YFBP質(zhì)量的主要化學(xué)成分。結(jié)果 15批YFBP基準(zhǔn)樣品HPLC指紋圖譜相似度>0.817;共歸屬30個(gè)特征峰,并指認(rèn)出8個(gè)特征峰信息,其中30號(hào)峰(亞油酸)為薏苡仁專屬峰;2(去甲豬毛菜堿)、9、22(苯甲酰新烏頭原堿)號(hào)峰為附子專屬峰;3(原兒茶酸)、4~6、7(綠原酸)、8、10(咖啡酸)、11、13、18、19、20(異綠原酸A)、21(異綠原酸C)、23~26號(hào)峰為敗醬草專屬峰;1、12、14~17、27~29號(hào)峰為薏苡仁和敗醬草共有特征峰;15批基準(zhǔn)樣品出膏率為20.06%~33.22%;指標(biāo)性成分原兒茶酸、綠原酸、咖啡酸、異綠原酸A、異綠原酸C、苯甲酰新烏頭原堿、亞油酸的質(zhì)量分?jǐn)?shù)分別為0.012~0.076、0.025~0.308、0.011~0.047、0.011~0.049、0.014~0.044、0.031~0.111、0.031~0.067 mg/g,轉(zhuǎn)移率分別為5.05%~30.86%、5.24%~21.31%、3.57%~43.22%、4.59%~18.69%、6.97%~23.13%、9.68%~62.32%、6.60%~19.95%;化學(xué)模式識(shí)別分析將15批樣品分為2類,OPLS-DA篩選出了導(dǎo)致質(zhì)量差異的14個(gè)特征峰,其中包括已被識(shí)別的峰3(原兒茶酸)、10(咖啡酸)、20(異綠原酸A)。結(jié)論 結(jié)合化學(xué)模式識(shí)別,建立了經(jīng)典名方Y(jié)FBP基準(zhǔn)樣品的HPLC指紋圖譜及多指標(biāo)性成分定量測(cè)定方法,并對(duì)其量值傳遞過程進(jìn)行分析,為YFBP基準(zhǔn)樣品的質(zhì)量控制及復(fù)方制劑開發(fā)提供了科學(xué)參考依據(jù)。
[Key word]
[Abstract]
Objective The HPLC fingerprints of the benchmark samples of the classic prescription Yiyi Fuzi Baijiang Powder (薏苡附子敗醬散, YFBP) was established, and the contents of its index components (protocatechuic acid, chlorogenic acid, caffeic acid, isochlorogenic acid A, isochlorogenic acid C, benzoylmesaconine and linoleic acid) were determined to study the quantitative value transfer pattern of YFBP and to evaluate its quality by combining with chemical pattern recognition to assess its quality. Methods By HPLC fingerprinting of 15 batches of YFBP benchmark samples, the common peaks and extraction yield range were identified, and the marker components were quantitatively determined. Simultaneously, hierarchical cluster analysis (HCA), principal component analysis (PCA), and orthogonal partial least squares-discriminant analysis (OPLS-DA) were employed to identify the key chemical components influencing the quality of YFBP. Results In 15 batches of YFBP benchmark samples, the HPLC fingerprint similarity was greater than 0.817. A total of 30 common peaks were identified, and eight common peaks were recognised, with specific attributions as follows: Peak 30 (linoleic acid) was specific to Yiyiren (Coicis Semen). Peaks 2 (salsolinol), 9, and 22 (benzoylmesaconine) were specific to Fuzi (Aconiti Lateralis Radix Praeparata). Peaks 3 (protocatechuic acid), 4—6, 7 (chlorogenic acid), 8, 10 (caffeic acid), 11, 13, 18, 19, 20 (isochlorogenic acid A), 21 (isochlorogenic acid C), 23—26 were specific to Baijiangcao (Patriniae Herba). Peaks 1, 12, 14—17, 27—29 were common to both Coicis Semen and Patriniae Herba. The extraction rate of the 15 batches ranged from 20.06% to 33.22%. The mass fraction of protocatechuic acid, chlorogenic acid, caffeic acid, isochlorogenic acid A, isochlorogenic acid C, benzoylmesaconine and linoleic acid were 0.012—0.076, 0.025—0.308, 0.011—0.047, 0.011—0.049, 0.014—0.044, 0.031—0.111, and 0.031—0.067 mg/g. Transfer rate were 5.05%—30.86%, 5.24%—21.31%, 3.57%—43.22%, 4.59%—18.69%, 6.97%—23.13%, 9.68%—62.32%, and 6.60%—19.95%. The chemometric analysis classified the 15 batches of samples into two groups, and OPLS-DA identified 14 common peaks responsible for quality differences. Among these, three peaks have been identified: peak 3 (protocatechuic acid), peak 10 (caffeic acid), and peak 20 (isochlorogenic acid A). Conclusion Based on chemical pattern recognition, an HPLC fingerprint and a multi-index component content determination method were established for the YFBP benchmark samples of a classical prescription. The process of quantitative transfer was analyzed, providing a scientific reference for quality control and the development of compound preparations based on YFBP standard samples.
[中圖分類號(hào)]
R283.6
[基金項(xiàng)目]
國(guó)家自然科學(xué)基金資助項(xiàng)目(82260847);貴州省科學(xué)技術(shù)廳科技創(chuàng)新人才團(tuán)隊(duì)(黔科合平臺(tái)人才-CXTD[2023]020);貴州省教育廳高校科技創(chuàng)新團(tuán)隊(duì)(黔教技[2023]069號(hào));貴州省科技計(jì)劃項(xiàng)目(黔科合基礎(chǔ)-ZK[2023]重點(diǎn)046);國(guó)家中醫(yī)藥管理局高水平中醫(yī)藥重點(diǎn)學(xué)科建設(shè)項(xiàng)目(zyyzdxk-2023185);貴州省基礎(chǔ)研究自然科學(xué)項(xiàng)目(黔科合基礎(chǔ)-ZK[2022]一般483)