摘要
目的 建立陈皮土(赤石脂)炒前后的HPLC指纹图谱及多成分定量测定方法,结合化学计量学进行比较,分析其特征指标成分,为陈皮及土(赤石脂)炒陈皮的质量控制和综合利用提供科学依据.方法 采用菲罗门Superlu C18色谱柱,流动相为乙腈-0.1％甲酸水溶液,梯度洗脱;体积流量1.0 mL/min;检测波长283 nm;柱温30℃;进样量10μL;HPLC法建立陈皮和土(赤石脂)炒陈皮的指纹图谱,运用相似度分析、主成分分析(principal component analysis,PCA)、正交偏最小二乘法-判别分析(orthogonal partial least squares-discriminant analysis,OPLS-DA)等化学模式识别技术,筛选出土(赤石脂)炒陈皮炮制前后特征指标成分并进行定量分析.结果 建立了陈皮和土(赤石脂)炒陈皮的HPLC指纹图谱,共提取出16个共有峰,通过与对照品对比,指认了6种成分,分别为辛弗林(1号峰)、芸香柚皮苷(10号峰)、橙皮苷(12号峰)、橙皮内酯(14号峰)、川陈皮素(15号峰)、橘皮素(16号峰);通过PCA和OPLS-DA可明显将陈皮和土(赤石脂)炒陈皮分为2类,综合筛选了辛弗林、芸香柚皮苷、橙皮苷、川陈皮素、橘皮素5种特征指标成分,炮制后辛弗林含量升高明显(P<0.01);芸香柚皮苷、橙皮苷、川陈皮素、橘皮素含量稍有降低.结论 确定了辛弗林、芸香柚皮苷、橙皮苷、川陈皮素、橘皮素5种特征指标成分作为评价陈皮及土(赤石脂)炒陈皮质量差异的潜在标志性成分,建立的陈皮及土(赤石脂)炒陈皮HPLC指纹图谱及多成分定量测定方法稳定、可靠,可为陈皮及土(赤石脂)炒陈皮的质量控制、综合利用和临床应用提供参考.
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.
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