树莓叶黄酮提取的正交试验和响应曲面法工艺优化对比
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摘要
旨在为树莓叶黄酮的开发应用提供数据参考,通过正交试验与响应曲面法设计改良乙醇提取工艺,并通过HPLC建立树莓叶黄酮的色谱分离条件为:Agilent ZorBax SB色谱柱,流动相为1 mg/mL乙酸-乙腈=72.5∶27.5,等度分离,柱温30℃,检测波长:257 nm,完成树莓叶黄酮的初步分离,以及黄酮中芦丁含量的准确测定和验证。最佳提取工艺为:646 mL/mL乙醇,料液比1∶12.5,41.9℃加热回流173.3 min,最佳工艺所得提取率1.127%,响应曲面法最佳工艺提取率略高于正交试验法,且其工艺条件均较优于正交试验所得工艺,可为后期研发树莓叶芦丁兽用中药制剂提供理论参考。
In order to provide data reference for the development and application of raspberry leaf flavonoids,this study designed the improved ethanol extraction process by orthogonal test and response surface method, and established the chromatographic separation conditions of raspberry leaf flavonoids by HPLC method:Agilent ZorBax SB chromatographic column,1 mg/mL acetic acid acetonitrile=72.5∶27.5,with isometric separation and column temperature 30 ℃,the detection wavelength:257 nm,completing the preliminary separation of flavonoids from raspberry leaves and the accurate determination of the content of rutin in flavonoids;The optimum extraction process is 646 mL/L ethanol,the ratio of the material to liquid 1∶12.5, and heatig refluxly for 173.3 min at the temperature of 41.9 ℃,and the extraction rate of raspberry leaf flavonoids is 1.127%.The optimum extraction rate of response surface method is slightly higher than that of orthogonal experiment,and the technological conditions are better than those obtained by orthogonal test,which can provide a theoretical reference for developing raspberry leaf rutin veterinary granules later.
In order to provide data reference for the development and application of raspberry leaf flavonoids,this study designed the improved ethanol extraction process by orthogonal test and response surface method, and established the chromatographic separation conditions of raspberry leaf flavonoids by HPLC method:Agilent ZorBax SB chromatographic column,1 mg/mL acetic acid acetonitrile=72.5∶27.5,with isometric separation and column temperature 30 ℃,the detection wavelength:257 nm,completing the preliminary separation of flavonoids from raspberry leaves and the accurate determination of the content of rutin in flavonoids;The optimum extraction process is 646 mL/L ethanol,the ratio of the material to liquid 1∶12.5, and heatig refluxly for 173.3 min at the temperature of 41.9 ℃,and the extraction rate of raspberry leaf flavonoids is 1.127%.The optimum extraction rate of response surface method is slightly higher than that of orthogonal experiment,and the technological conditions are better than those obtained by orthogonal test,which can provide a theoretical reference for developing raspberry leaf rutin veterinary granules later.
引文
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[2] 王倩倩.树莓叶果中水杨酸含量评价及抑菌性分析[D].黑龙江哈尔滨:东北农业大学,2014.
[3] 魏小聪,赵艳敏,崔雨,等.HPLC法测定树莓叶和果实中鞣花酸的含量[J].武警后勤学院学报:医学版,2016,25(1):29-31.
[4] 刘卉,杨国伟,兰蓉,等.树莓叶中鞣花酸提取工艺的研究[J].食品研究与开发,2015,36(18):55-58.
[5] 吴士龙,李敏,李小玢,等.响应曲面法优化树莓叶中鞣花酸的提取工艺[J].中国新药杂志,2014,23(6):692-697.
[6] 张雨昕.树莓叶黄酮类物质的提取及其抗氧化活性研究[D].天津:天津科技大学,2012.
[7] 叶晓珂.树莓叶黄酮类活性成分的分离与鉴定研究[D].天津:天津科技大学,2011.
[8] 陈晓慧.树莓叶中黄酮类化合物的提取、分离及结构鉴定的研究[D].黑龙江哈尔滨:东北农业大学,2007.
[9] 臧慧明,吴林,张强,等.树莓籽与树莓叶副产物的开发进展[J].食品工业科技,2017(24):325-330.
[10] 杨国慧,张岩,于洋,等.树莓叶果黄酮类化合物含量及抗氧化性分析[J].湖北农业科学,2015(18):4514-4518.
[11] 李敏.槲皮素及其糖苷衍生物芦丁对心肌纤维化的抑制作用及机制研究[D].吉林长春:吉林大学,2014.
[12] 徐雅琴,于泽源,任华锋.红树莓叶片中黄酮类物质提取及抗氧化性的研究[J].中国油脂,2003(5):69-71.