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高纯橙皮素的制备及HPLC纯度分析
引用本文:李珍柱,焦必宁,王敏,周剑,苏学素.高纯橙皮素的制备及HPLC纯度分析[J].分析测试学报,2017,36(12):1500-1505.
作者姓名:李珍柱  焦必宁  王敏  周剑  苏学素
作者单位:1.西南大学化学化工学院;2.中国农业科学院/西南大学柑桔研究所,农业部柑桔产品质量安全 风险评估实验室(重庆);3.中国农业科学院农业质量标准与检测技术研究所
基金项目:国家现代农业(柑桔)产业技术体系建设专项(CARS-26);国家重点研发专项(2016YFF0201105-2);国家农产品质量安全风险评估重大专项(GJFP2017004,GJFP2017015)
摘    要:建立了一种基于反相硅胶纯化的高纯橙皮素制备方法,充分优化了上样量、流速及洗脱液极性等因素,采用红外光谱法和核磁共振对纯化后产物进行定性分析,高效液相色谱法检测纯化前后橙皮素的纯度,最终产物的纯度达99.87%。该方法快速简便、制备量大、分离效率高,每天制备效率可达到克级,为制备橙皮素标准物质提供了技术支撑。

关 键 词:橙皮素  反相硅胶  纯化  定性分析  高效液相色谱

Preparation of Hesperetin Based on Reversed Phase Silica Gel Purification and Its Purity Analysis by HPLC
LI Zhen-zhu,JIAO Bi-ning,WANG Min,ZHOU Jian,SU Xue-su.Preparation of Hesperetin Based on Reversed Phase Silica Gel Purification and Its Purity Analysis by HPLC[J].Journal of Instrumental Analysis,2017,36(12):1500-1505.
Authors:LI Zhen-zhu  JIAO Bi-ning  WANG Min  ZHOU Jian  SU Xue-su
Abstract:In this study,a method for the preparation of high purity hesperetin based on reversed-phase silica gel purification was established.The factors such as loading volume,flow rate and eluent polarity were optimized.Structure of the product was identified by infrared spectroscopy and nuclear magnetic resonance,and the purity of the analyte was 99.87%.The daily preparation efficiency of the method could reach to gram-grade.With the advantages of high efficiency,large preparation and high separation efficiency,the method could provide a technical support for the preparation of certified reference material of hesperetin.
Keywords:hesperetin  reverse phase silica gel  purification  qualitative analysis  high performance liquid chromatography
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