Cvek J, Medić-Sarić M, Jasprica I, Zubcić S, Vitali D, Mornar A, Vedrina-Dragojević I, Tomić S
Agency for Medicinal Products and Medical Devices, Ksaverska cesta 4, 10000 Zagreb, Croatia.
Phytochem Anal. 2007 Sep-Oct;18(5):451-9. doi: 10.1002/pca.1001.
Three spectrophotometric methods for the quantitative determination of different flavonoid groups and total phenolics in Croatian propolis samples were optimised and validated. The assay based on the formation of aluminium chloride complex (with galangin as a standard) was applied to the quantification of flavones and flavonols, while the 2,4-dinitrophenylhydrazine method (with pinocembrine as a reference) was used for the quantification of flavanones. Total phenolic content was measured by the Folin-Ciocalteau method using reference solution of caffeic acid:galangin:pinocembrine (1:1:1). Through analytical validation, the most suitable extraction conditions (with respect to time, temperature and concentration of extraction solvent) were determined, and final conditions for the extraction were established (80% ethanol, 1 h at the room temperature). The appropriate ratio between the mass of raw propolis and the extraction solvent volume was also established. By the application of the optimised method of extraction, 10 propolis tinctures were prepared and subjected to the analysis of general pharmacopoeial parameters, which are fundamental for the creation of quality specification (relative density, dry residue of extract, content of ethanol, methanol and 2-propanol). Additionally, the content of waxes as the main inactive constituents was determined in order to observe the level of their migration from crude propolis to the prepared tinctures.
对三种用于定量测定克罗地亚蜂胶样品中不同类黄酮基团和总酚含量的分光光度法进行了优化和验证。基于氯化铝络合物形成的测定法(以高良姜素为标准品)用于黄酮和黄酮醇的定量,而2,4-二硝基苯肼法(以松属素为参比)用于黄烷酮的定量。总酚含量通过福林-西奥尔特法测定,使用咖啡酸:高良姜素:松属素(1:1:1)的参比溶液。通过分析验证,确定了最合适的提取条件(关于时间、温度和提取溶剂浓度),并确定了最终的提取条件(80%乙醇,室温下1小时)。还确定了生蜂胶质量与提取溶剂体积之间的合适比例。通过应用优化的提取方法,制备了10种蜂胶酊剂,并对一般药典参数进行了分析,这些参数是制定质量标准的基础(相对密度、提取物干残渣、乙醇、甲醇和2-丙醇含量)。此外,测定了作为主要非活性成分的蜡的含量,以观察其从粗蜂胶向制备的酊剂中的迁移水平。