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目的:优选山核桃树皮中槲皮苷的提取工艺,并建立其含量测定方法。方法:采用乙醇回流法提取山核桃树皮,经聚酰胺吸附去杂、多次析晶得槲皮苷,采用核磁共振波谱法(NMR)确证其结构,HPLC测定其含量。通过正交试验考察乙醇体积分数、提取时间和提取次数对槲皮苷得率的影响。结果:经NMR确证产物为槲皮苷,HPLC表明其在4.8～91.2 mg·L-1呈良好线性关系,山核桃树皮中槲皮苷含量高达8.37%。最佳提取工艺为10倍量60%乙醇回流提取2次,每次1 h,提取率>90%。结论:建立的山核桃中槲皮苷含量测定方法简单精确,优选的提取工艺稳定可行。
Objective: To optimize the extraction process of quercitrin in bark of pecan tree and to establish a method for its determination. Methods: The bark of Hickory bark was extracted by ethanol reflux method. The polysaccharides were separated by polyamides to obtain quercetin. The structures of the samples were confirmed by nuclear magnetic resonance (NMR) and the content was determined by HPLC. The effects of ethanol volume fraction, extraction time and extraction times on the yield of quercetin were investigated by orthogonal test. Results: The product was confirmed to be quercetin by NMR. HPLC showed a good linear relationship with 4.8 ~ 91.2 mg · L-1, and the content of quercitrin in bark of pecan was as high as 8.37%. The best extraction process is 10 times the amount of 60% ethanol reflux extraction 2 times, each 1 h, extraction rate> 90%. Conclusion: The method for determination of quercetin in pecan was simple and accurate, and the optimal extraction process was stable and feasible.