天然富硒植物无花果叶中硒提取方法的研究

李军德, 刘晓娟, 宋吉英

doi:10.3969/j.issn.1006-267x.2019.03.055

动物营养学报 >

2019 , Vol. 31 >Issue 3: 1463 - 1470

DOI: https://doi.org/10.3969/j.issn.1006-267x.2019.03.055

研究简报 Short Communications

天然富硒植物无花果叶中硒提取方法的研究

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1. 青岛农业大学校医院, 青岛 266109;
2. 青岛农业大学化学与药学院, 青岛 266109

李军德(1969-),男,山东烟台人,主治医师,学士,从事药物分析研究。E-mail:junde68@163.com

收稿日期: 2018-08-27

网络出版日期: 2019-03-18

基金资助

国家自然科学基金项目（21775083）；国家级大学生科技创新训练项目（201810435065）

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Study on Extraction Methods of Selenium in Fig Leaves as a Natural Selenium-Enriched Plant

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1. Hospital of Qingdao Agricultural University, Qingdao 266109, China;
2. College of Chemistry and Pharmaceutical Sciences, Qingdao Agricultural University, Qingdao 266109, China

Received date: 2018-08-27

Online published: 2019-03-18

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摘要

本试验旨在比较天然富硒植物无花果叶中硒的提取方法。试验采用4种方法从无花果叶中提取硒，分别是混合酸消解法、超声-微波协同萃取法、索氏提取法和磁力搅拌法，讨论每种方法的不同提取条件对提取效果的影响，并将提取到的硒用灵敏度高的荧光光度法进行定量。结果表明：1）混合酸消解法提取硒的效果最好，超声-微波协同萃取法提取效果略次之，磁力搅拌法提取硒的效果最差。2）混合酸消解法4种不同的混合酸消解体系中，高氯酸-硫酸-硝酸（体积比1：1：3）组成的消解体系提取硒的效果最好，消解24 h提取硒的含量为0.13 μg/g。3）正交试验确定超声-微波协同萃取法的最佳提取条件是用甲醇作为提取剂，微波功率400 W，提取时间15 min，物料比1：10（g：mL），在此条件下提取硒的含量为0.12 μg/g。由此可知，不同方法提取无花果叶中硒的效果不同。混合酸消解法虽然提取硒的效果最好，但是该方法中用的强酸危险性大，试验周期长；超声-微波协同萃取法提取硒的效果仅略差于混合酸消解法，同时该方法可实时监控，操作简单安全，且试验耗时远远低于混合酸消解法。因此，建议采用超声-微波协同萃取法提取无花果叶中的硒。

关键词： 硒; 无花果叶; 提取方法; 荧光

本文引用格式

李军德, 刘晓娟, 宋吉英 . 天然富硒植物无花果叶中硒提取方法的研究[J]. 动物营养学报, 2019 , 31(3) : 1463 -1470 . DOI: 10.3969/j.issn.1006-267x.2019.03.055

Abstract

This experiment was conducted to compare the extraction method of selenium from fig leaves which had rich selenium as a natural plant. The four extraction methods, including mixed acid digestion method, ultrasound-microwave synergistic extraction method, Soxhlet extraction method and magnetic stirring method were discussed and evaluated. The different conditions for extraction efficiency were optimized and selenium content in fig leaves was measured by fluorescence spectrometry with high sensitivity. The results showed as follows:1) the mixed acid digestion method had the highest extraction efficiency, the ultrasound-microwave synergistic extraction method was slightly worse than the mixed acid digestion method, and the magnetic stirring method was the worst. 2) In the four different acid digestion systems of mixed acid digestion method, the system consisting of the volume ratio of perchloric acid, sulphuric acid and nitric acid was 1:1:3 had the best effect for extracting selenium. The content of selenium in fig leaves was 0.13 μg/g with extraction time 24 h. 3) The content of selenium was 0.12 μg/g with ultrasound-microwave synergistic extraction method. The optimum extraction conditions of ultrasound-microwave synergistic extraction method through orthogonal test were identified as the follows:methanol as solvent, microwave power 400 W, extraction time 15 min and solid-liquid ratio as 1:10 (g:mL). The results indicated that there are differences of extraction effect with different methods. The mixed acid digestion method has the best extraction effect but strong acids used in the experiment is too dangerous for the operation with long time digestion. The extraction effect of ultrasound-microwave synergistic extraction method is slightly worse than the mixed acid digestion method, but it can shorten extraction time, reduce sample consumption, operate expediently and monitor in real time. Therefore, ultrasound-microwave synergistic extraction method for extracting selenium from fig leaves is recommended.

Key words： selenium; fig leaves; extraction method; fluorescence

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