该研究建立了化橘红(Citrus grandis cv. ‘Tomentosa’)果实中4种类黄酮成分的提取分离、HPLC定量和指纹图谱分析方法, 利用该方法测定了果实生长发育过程中类黄酮的动态变化。结果表明, 用60%乙醇超声辅助提取果实干燥粉末2小时, 柚皮苷提取率达到98%以上。用HPLC分离和测定提取物中柚皮苷、野漆树苷、柚皮素和芹菜素的含量及其指纹图谱。结果显示, 15–60天不同果龄的果实中类黄酮含量(占果实干重)随着果龄的增大而降低, 柚皮苷、野漆树苷、柚皮素和芹菜素分别从52.5%、0.74%、0.57%和0.23%降低至16.1%、0.11%、0.06%和0.03%; 每果中类黄酮总量则随着果龄的增加而大幅提高, 从15天的0.55 g提高至60天的7.99 g。上述研究结果表明, 果龄对化橘红类黄酮含量、产量及药材质量均有很大的影响。该研究为化橘红的工业生产和质量监控提供了重要依据。
Citrus grandis cv. ‘Tomentosa’ is an important traditional Chinese medicine agent; naringin and other flavonoids are the main functional and quality control compounds. We established methods for extraction, high-performance liquid chromatography (HPLC) quantitative and fingerprint analyses of flavonoid content of C. grandis cv. ‘Tomentosa’ and analyzed dynamic changes in content during fruit growth and development. The powder from fruit was extracted with 60% ethanol for 2 h by ultrasound-assisted maceration extraction. The extraction of naringin reached ≥98%. Separation and quantitative determination of flavoloids and fingerprint analysis of extracts by HPLC involved Thermo C18 columns and a gradient eluent of 35% to 65% acidic methanol. Content of the 4 main flavonoids was analyzed every 5 days from days 15 to 60. Total flavonoid content increased significantly with fruit age from 0.55 to 7.99 g·fruit–1. However, on a fruit dry-weight basis, content of flavonoid decreased significantly with fruit age and that of naringin from 52.5% to 16.1%, rhoifolin from 0.74% to 0.11%, naringenin from 0.57% to 0.06%, and apigenin from 0.23% to 0.03%. Fruit age had a great impact on fruit flavonoid content, yield and quality of medicinal material from fruit. We provide important information for industrial production and quality control of C. grandis cv. ‘Tomentosa’.
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