[關(guān)鍵詞]
[摘要]
目的 建立陳皮土(赤石脂)炒前后的HPLC指紋圖譜及多成分定量測(cè)定方法,結(jié)合化學(xué)計(jì)量學(xué)進(jìn)行比較,分析其特征指標(biāo)成分,為陳皮及土(赤石脂)炒陳皮的質(zhì)量控制和綜合利用提供科學(xué)依據(jù)。方法 采用菲羅門Superlu C18色譜柱,流動(dòng)相為乙腈-0.1%甲酸水溶液,梯度洗脫;體積流量1.0 mL/min;檢測(cè)波長(zhǎng)283 nm;柱溫30 ℃;進(jìn)樣量10μL;HPLC法建立陳皮和土(赤石脂)炒陳皮的指紋圖譜,運(yùn)用相似度分析、主成分分析(principal component analysis,PCA)、正交偏最小二乘法-判別分析(orthogonal partial least squares-discriminant analysis,OPLS-DA)等化學(xué)模式識(shí)別技術(shù),篩選出土(赤石脂)炒陳皮炮制前后特征指標(biāo)成分并進(jìn)行定量分析。結(jié)果 建立了陳皮和土(赤石脂)炒陳皮的HPLC指紋圖譜,共提取出16個(gè)共有峰,通過與對(duì)照品對(duì)比,指認(rèn)了6種成分,分別為辛弗林(1號(hào)峰)、蕓香柚皮苷(10號(hào)峰)、橙皮苷(12號(hào)峰)、橙皮內(nèi)酯(14號(hào)峰)、川陳皮素(15號(hào)峰)、橘皮素(16號(hào)峰);通過PCA和OPLS-DA可明顯將陳皮和土(赤石脂)炒陳皮分為2類,綜合篩選了辛弗林、蕓香柚皮苷、橙皮苷、川陳皮素、橘皮素5種特征指標(biāo)成分,炮制后辛弗林含量升高明顯(P<0.01);蕓香柚皮苷、橙皮苷、川陳皮素、橘皮素含量稍有降低。結(jié)論 確定了辛弗林、蕓香柚皮苷、橙皮苷、川陳皮素、橘皮素5種特征指標(biāo)成分作為評(píng)價(jià)陳皮及土(赤石脂)炒陳皮質(zhì)量差異的潛在標(biāo)志性成分,建立的陳皮及土(赤石脂)炒陳皮HPLC指紋圖譜及多成分定量測(cè)定方法穩(wěn)定、可靠,可為陳皮及土(赤石脂)炒陳皮的質(zhì)量控制、綜合利用和臨床應(yīng)用提供參考。
[Key word]
[Abstract]
Objective To establish HPLC fingerprint and multi-component content determination method of Chenpi (Citri Reticulatae Pericarpium, CRP) before and after soil-stir-baked with Chishizhi (Halloysitum Rubrum, HR), and to analyze its characteristic index components combined with chemometrics, so as to provide scientific basis for quality control and comprehensive utilization of CRP and canned products. Methods The chromatography was performed on Superlu C18 column with acetonitrile-0.1% formic acid aqueous solution as mobile phase and gradient elution. Volume flow rate 1.0 mL/min; The detection wavelength was 283 nm. Column temperature 30 ℃; The sample size was 10 μL. The fingerprints of CRP and fried soil-stir-baked CRP with HR were established by HPLC. Similarity analysis, principal component analysis (PCA), orthogonal partial least squares-discriminant analysis (OPLS-DA) and other chemical pattern recognition techniques were used to screen the characteristic components of CRP before and after processing, and quantitative analysis was carried out. Results The fingerprints of CRP and fried soil-stir-baked CRP with HR were established, 16 common peaks were extracted, and six components were identified by comparing with the control products, namely, syneferine (peak 1), naringin (peak 10), hesperidin (peak 12), hesperidin (peak 14), nobiletin (peak 15) and tangeretin (peak 16). CRP and fried soil-stir-baked CRP with HR could be divided into two categories by PCA and OPLS-DA. Five characteristic components, synephrine, naringin, hesperidin, nobiletin and tangeretin, were screened. After processing, the contents of ariephrin and synephrin increased, and the content of synephrin increased significantly (P < 0.01). The contents of hesperidin, nobiletin and tangeretin decreased slightly. Conclusion Five characteristic components, syneferin, naringin, nobiletin, tangeretin, were identified as potential landmark components to evaluate the quality difference between CRP and fried soil-stir-baked CRP with HR. The established HPLC fingerprint and multi-component content determination method of CRP and fried soil-stir-baked CRP with HR were stable and reliable, and could provide reference for quality control, comprehensive utilization and clinical application of CRP and its prepared products.
[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(82060724);建昌幫特色飲片陳皮(蒸)等9味炮制規(guī)范和質(zhì)量標(biāo)準(zhǔn)研究(橫20220362);江西省中醫(yī)藥標(biāo)委會(huì)2021年第二批標(biāo)準(zhǔn)化項(xiàng)目(2021B01);江西省中醫(yī)藥標(biāo)委會(huì)2021年第二批標(biāo)準(zhǔn)化項(xiàng)目(2023A19);大學(xué)生創(chuàng)新創(chuàng)業(yè)訓(xùn)練計(jì)劃項(xiàng)目(202310412027);大學(xué)生創(chuàng)新創(chuàng)業(yè)訓(xùn)練計(jì)劃項(xiàng)目(S202310412061)