CN106770823A - 利用磁性石墨烯吸附人参饮料中皂苷Rg1、Re的方法 - Google Patents
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Abstract
本发明公开了利用磁性石墨烯吸附人参饮料中皂苷Rg1、Re的方法。取30mL花旗参饮料和20mg石墨烯加入到50mL离心管，在室温下放置到振荡器上振摇40分钟，吸附结束后将一块磁铁放到试管外壁，将试管内溶液弃去。用2mL环己烷将沉淀物转移到15mL的试管中，涡旋淋洗，然后再用磁铁将磁性石墨烯与环己烷溶液分离，再加入8mL甲醇，超声20分钟后，用磁铁将石墨烯吸附，用5mL注射器收集剩余溶液，经0.4μm微孔滤膜过滤，用氮气吹干，再加200μL甲醇复溶，取10μL注入高效液相色谱分析测定吸附量。
Description
技术领域
本发明设计一种吸附人参饮料中的常见皂苷Rg1、Re的新方法，属于精细化工技术领域。
背景技术
人参是应用历史最为久远的名贵药用植物，其药用价值早为世人所公认。《神农本草经》中记载“主补五脏、安精神、定魂魄、止惊悸、除邪气、明目开心益智，久服轻身延年”。随着人参栽培技术的成熟，人参属植物资源得以丰富，人参从奢侈品变为普通消费品，人参保健品也由此产生。人参的主要活性成分是人参皂苷，每种人参皂苷都有其独特的生理活性。大量的研究结果表明，人参皂苷具有抗氧化、抗肿瘤、提高机体免疫力、抑制细胞凋亡等药理活性。参皂苷是人参中主要的功效成分，其中含量较高的人参皂苷主要有Rb1、Rb2、Rc、Rd、Re、Rg1等。
人参软饮料的主要原料是饮用水或矿泉水，果汁、蔬菜汁或植物的根、茎、叶、花和果实的抽提液。有的含甜味剂、酸味剂、香精、香料、食用色素、乳化剂、起泡剂、稳定剂和防腐剂等食品添加剂。其基本化学成分是水分、碳水化合物和风味物质，有些软饮料还含维生素和矿物质。本实验主要测定人参饮料中常见人参皂苷Rg1,Re的含量。
磁性固相萃取是将吸附材料分散在样品溶液中直接吸附目标物的一种样品处理技术，具有样品与吸附剂接触充分、传质速率速度快，分析时间短、萃取效率高等优点，被广泛应用在药物载体、细胞分离、酶固定、生物传感器等诸多领域。由于磁性石墨烯材料具有化学稳定性好、比表面积大等优异的物化性能，作为吸附剂在样品前处理中展现了良好的应用前景。
发明内容
本发明是为了解决常规方法测定人参饮料中的常见皂苷Rg1、Re时，测定耗时长，操作复杂，使用有毒有害有机试剂多等缺点，利用磁性石墨烯的吸附能力强的特点，将人参饮料中的常见皂苷Rg1、Re吸附在磁性石墨烯上。
本发明的技术方案由以下部分组成。
(1)磁性石墨烯对人参饮料中常见皂苷Rg1、Re的吸附
取50mL花旗参饮料和20mg石墨烯加入到50mL离心管，在室温下放置到振荡器上振摇40分钟，吸附结束后将一块磁铁放到试管外壁，将试管内溶液弃去。
(2)淋洗除去杂质
用2mL环己烷将沉淀物转移到5mL的试管中，涡旋淋洗，然后再用磁铁将磁性石墨烯与环己烷溶液分离。
(3)对中常见皂苷Rg1、Re的洗脱
在淋洗后的石墨烯中加入2mL甲醇，超声20分钟后，用磁铁将石墨烯吸附，用5mL注射器收集剩余溶液，经0.4μm微孔滤膜过滤，用氮气吹干，再加200μL甲醇复溶，取10μL注入高效液相色谱分析。
本实验选用磁性石墨烯为吸附剂，由于磁性石墨烯具有石墨烯良好的吸附性，所以能很好的吸附人参饮料中常见皂苷Rg1、Re，同时磁性石墨烯具有磁性，所以使得吸附洗脱的过程变得更为简单易行。
下面结合实例对本发明内容进行描述。
附图说明
图1是常见人参皂苷Re、Rg1标准品的色谱图(标准品浓度为1mg/mL)；
图2是实施例1的色谱图；
图3是实施例2的色谱图；
图4是实施例3的色谱图；
具体实施例
实施例1
将30mL花旗参饮料和20mg磁性石墨烯加入到50mL离心管，在室温下放置到摇床上分别振荡40min，吸附结束后，将一块磁铁放到50mL离心管外壁，将试管内溶液弃去，分别用2mL的环己烷振荡淋洗，转移到15mL离心机管中，然后再用磁铁将吸附剂与淋洗剂分离。加入8mL甲醇，超声20分钟洗脱，超声结束后，用磁铁将吸附剂与洗脱剂分离，用5mL注射器吸取洗脱剂，经0.4μm微孔滤膜过滤，用氮吹仪吹干，加入200μL的色谱甲醇复溶，取10μL注入高效液相色谱。
经上述方法获得的人参饮料中的常见皂苷Rg1、Re的吸附量分别为0.0476mg/mL和0.0586mg/mL。
实施例2
将10mL花旗参饮料和20mg磁性石墨烯加入到50mL离心管，在室温下放置到摇床上分别振荡40min，吸附结束后，将一块磁铁放到50mL离心管外壁，将试管内溶液弃去，分别用2mL的环己烷振荡淋洗，转移到15mL离心机管中，然后再用磁铁将吸附剂与淋洗剂分离。加入8mL甲醇，超声20分钟洗脱，超声结束后，用磁铁将吸附剂与洗脱剂分离，用5mL注射器吸取洗脱剂，经0.4μm微孔滤膜过滤，用氮吹仪吹干，加入200μL的色谱甲醇复溶，取10μL注入高效液相色谱。
经上述方法获得的人参饮料中的常见皂苷Rg1、Re的吸附量分别为0.0336mg/mL和0.0323mg/mL。
实施例3
将50mL花旗参饮料和20mg磁性石墨烯加入到50mL离心管，在室温下放置到摇床上分别振荡40min，吸附结束后，将一块磁铁放到50mL离心管外壁，将试管内溶液弃去，分别用2mL的环己烷振荡淋洗，转移到15mL离心机管中，然后再用磁铁将吸附剂与淋洗剂分离。加入8mL甲醇，超声20分钟洗脱，超声结束后，用磁铁将吸附剂与洗脱剂分离，用5mL注射器吸取洗脱剂，经0.4μm微孔滤膜过滤，用氮吹仪吹干，加入200μL的色谱甲醇复溶，取10μL注入高效液相色谱。
经上述方法获得的人参饮料中的常见皂苷Rg1、Re的吸附量分别为0.013325mg/mL和0.039406mg/mL。
Claims (2)
1.利用磁性石墨烯吸附人参饮料中皂苷Rg1、Re的方法，其特征是，包括步骤如下：
(1)取30mL花旗参饮料和20mg石墨烯加入到50mL离心管，在室温下放置到振荡器上振摇40分钟，吸附结束后将一块磁铁放到试管外壁，将试管内溶液弃去；
(2)用2mL环己烷将沉淀物转移到15mL的试管中，涡旋淋洗，然后再用磁铁将磁性石墨烯与环己烷溶液分离；
(3)再加入8mL甲醇，超声20分钟后，用磁铁将石墨烯吸附，用5mL注射器收集剩余溶液，经0.4μm微孔滤膜过滤，用氮气吹干，再加200μL甲醇复溶，取10μL注入高效液相色谱分析。
2.根据权利要求1所述的利用磁性石墨烯吸附人参饮料中皂苷Rg1、Re的方法，其特征是洗脱剂为甲醇、洗脱剂体积8mL、提取时间40分钟、料液比2:3。
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| CN106226424A (zh) * | 2016-07-15 | 2016-12-14 | 山东畜牧兽医职业学院 | 一种磁性石墨烯固相萃取结合液质联用仪检测肉制品中兽药残留的方法 |
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