CN115090001B - 一种适用于颗粒材料搅拌萃取的萃取装置及其使用方法 - Google Patents
一种适用于颗粒材料搅拌萃取的萃取装置及其使用方法 Download PDFInfo
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Abstract
本发明属于磁固相萃取技术领域,本发明提供了一种适用于颗粒材料搅拌萃取的萃取装置及其使用方法。该萃取装置包括搅拌室、吸附萃取室和微孔滤膜,其使用方法包括以下步骤:在吸附萃取室中加入磁性吸附剂;用热熔胶将微孔滤膜固定在搅拌室和吸附萃取室的交接处;向萃取装置中添加含有分析物的液体;在搅拌室中放入搅拌子,进行搅拌萃取。本发明提出了将搅拌子与萃取所使用的磁性吸附剂分隔开来的方法,并利用搅拌进行萃取,解决了搅拌子在搅拌时极易吸附磁性吸附剂的问题,提升了萃取效率。
Description
技术领域
本发明涉及磁固相萃取技术领域,尤其涉及一种适用于颗粒材料搅拌萃取的萃取装置及其使用方法。
背景技术
目前,在进行萃取操作时,常用的方法为震荡法,但是其存在着萃取效率较低,富集倍数较低,且操作不够简便等技术缺陷。而在进行磁固相萃取时,可以使用搅拌子来加速目标物在吸附剂与溶剂之间的分配平衡,以此来增大萃取效率。但是,当使用搅拌子时,磁性吸附剂极易被吸附在搅拌子上,难以将磁性吸附剂与搅拌子完全分离,导致后续萃取效率降低。萃取完成后磁性吸附剂的解吸也难以操控。
因此,如何提供一种操作方法简便,萃取效率高的萃取装置及其使用方法成为了本领域技术人员亟需解决的问题。
发明内容
有鉴于此,本发明提供了一种适用于颗粒材料搅拌萃取的萃取装置及其使用方法。其目的是解决搅拌子在搅拌时极易吸附磁性吸附剂的问题,从而提升萃取效率。
为了达到上述目的,本发明采用如下技术方案:
本发明提供了一种适用于颗粒材料搅拌萃取的萃取装置,包括搅拌室、吸附萃取室和微孔滤膜;
所述搅拌室位于吸附萃取室的上方,微孔滤膜位于搅拌室和吸附萃取室的交接处;
所述微孔滤膜的直径大于搅拌室和吸附萃取室的交接处的中部瓶颈的直径。
进一步的,所述搅拌室中放入搅拌子,搅拌子的长度小于搅拌室和吸附萃取室的交接处的中部瓶颈的直径。
进一步的,所述吸附萃取室内放置磁性吸附剂。
本发明提供了上述萃取装置的使用方法,包括以下步骤:
在吸附萃取室中加入磁性吸附剂;用热熔胶将微孔滤膜固定在搅拌室和吸附萃取室的交接处;向萃取装置中添加含有分析物的液体;在搅拌室中放入搅拌子,进行搅拌萃取。
进一步的,向萃取装置中添加含有分析物的液体时,利用洗耳球增大搅拌室压强,克服搅拌室与吸附萃取室的压强差,从而使液体顺利进入吸附萃取室与磁性吸附剂接触。
经由上述的技术方案可知,与现有技术相比,本发明的有益效果如下:
本发明提供的萃取装置及其使用方法与震荡法相比,明显提高了萃取效率;本发明的技术方案解决了磁固相萃取时,搅拌子极易吸附磁性吸附剂的问题,并且提高了后续的萃取效率,还解决了搅拌子与磁性吸附剂难以分离、难以完全将磁性纳米颗粒所吸附的目标物质洗脱、难以计算萃取率等问题。
附图说明
图1为本发明提供的萃取装置的整体结构示意图,其中,1为搅拌室、2为吸附萃取室、3为微孔滤膜、4为搅拌子、5为磁性吸附剂;
图2为本发明提供的萃取装置的尺寸图。
具体实施方式
本发明提供了萃取装置的使用方法,包括以下步骤:
在吸附萃取室中加入磁性吸附剂;用热熔胶将微孔滤膜固定在搅拌室和吸附萃取室的交接处;向萃取装置中添加含有分析物的液体;在搅拌室中放入搅拌子,进行搅拌萃取。
在本发明中,所述微孔滤膜优选为PTFE微孔滤膜。
本发明提供的萃取装置的尺寸图如图2所示,利用此萃取装置进行萃取时,含有分析物的液体的添加量为40~60mL,优选为45~55mL,进一步优选为50mL。
在本发明中,用热熔胶将微孔滤膜固定在搅拌室和吸附萃取室的交接处,此时吸附萃取室不与外界大气压连通,只能通过微孔滤膜与搅拌室交换气体分子与液体内的分子、离子。
下面将对本发明实施例中的技术方案进行清楚、完整地描述,显然,所描述的实施例仅仅是本发明一部分实施例,而不是全部的实施例。基于本发明中的实施例,本领域普通技术人员在没有做出创造性劳动前提下所获得的所有其他实施例,都属于本发明保护的范围。
实施例1
(1)称取50mg磁性颗粒并置于吸附萃取室内;
(2)使用热熔胶将PTFE微孔滤膜粘在搅拌室与吸附萃取室中间;
(3)分别向该装置内加入50mL样品溶液,使萃取标准溶液的浓度分别为0.1mg/L、0.2mg/L、0.4mg/L、0.6mg/L、10mg/L、20mg/L,进行萃取标准曲线的建立;
(4)向搅拌室内放置一个直径为1.5cm的搅拌子;
(5)将该装置置于磁力搅拌器上搅拌1小时;
(6)将装置从磁力搅拌器上取下后静置一分钟,后使用磁铁将磁性颗粒吸附在吸附萃取室内,然后除去水相;
(7)向吸附萃取室内加入2mL正己烷,超声解吸15分钟;
(8)解吸完成后,取0.5mL液体于一圆底烧瓶中,用氮气将烧瓶内正己烷吹干,后加入0.5mL色谱甲醇,超声处理两分钟,使多氯联苯溶解到色谱甲醇中;
(9)使用高效液相色谱分析上清液;
(10)液相色谱条件:采用C18柱,流动相为乙腈/水=90/10(v/v),柱温为25℃,流速为1mL/min,检测波长为254nm;
(11)分别用高效液相色谱检测后,得到各个浓度的萃取液所对应的峰面积,分别做三氯联苯和六氯联苯的峰面积-浓度曲线,即其萃取标准曲线。
结果显示:三氯联苯的萃取标准曲线方程为:y=0.2955C+0.2728,R=0.9942;六氯联苯的萃取标准曲线方程为:y=0.6207C+0.6322,R=0.9778。
实施例2
(1)称取50mg磁性颗粒置于吸附萃取室内;
(2)使用热熔胶将PTFE微孔滤膜粘在搅拌室与吸附萃取室中间;
(3)向该装置内加入50mL含有未知浓度三氯联苯和六氯联苯的样品溶液;
(4)向搅拌室内放置一个直径为1.5cm的搅拌子;
(5)将该装置置于磁力搅拌器上搅拌萃取1小时;
(6)将装置从磁力搅拌器上取下后静置一分钟,后使用磁铁将磁性颗粒吸附在吸附萃取室内,然后除去水相;
(7)向吸附萃取室内加入2mL正己烷,超声解吸15分钟;
(8)解吸完成后,取0.5mL液体于一圆底烧瓶中,用氮气将烧瓶内正己烷吹干,后加入0.5mL色谱甲醇,超声处理两分钟,使多氯联苯溶解到色谱甲醇中;
(9)使用高效液相色谱分析上清液;
(10)液相色谱条件:采用C18柱,流动相为乙腈/水=90/10(v/v),柱温为25℃,流速为1mL/min,检测波长为254nm。
(11)分析结果表明:样品中三氯联苯的浓度为0.1mg/L、六氯联苯的浓度为0.1mg/L。
实施例3
(1)称取50mg磁性颗粒置于吸附萃取室内;
(2)使用热熔胶将PTFE微孔滤膜粘在搅拌室与吸附萃取室中间;
(3)再向该装置内加入50mL含有未知浓度三氯联苯和六氯联苯的样品溶液,其溶液的离子强度为25%的NaCl溶液;
(4)向搅拌室内放置一个直径为1.5cm的搅拌子;
(5)将该装置置于磁力搅拌器上搅拌1小时;
(6)将装置从磁力搅拌器上取下后静置一分钟,后使用磁铁将磁性颗粒吸附在吸附萃取室内,然后除去水相;
(7)向吸附萃取室内加入2mL正己烷,超声解吸15分钟;
(8)解吸完成后,取0.5mL液体于一圆底烧瓶中,用氮气将烧瓶内正己烷吹干,后加入0.5mL色谱甲醇,超声处理两分钟,使多氯联苯溶解到色谱甲醇中;
(9)使用高效液相色谱分析上清液;
(10)液相色谱条件:采用C18柱,流动相为乙腈/水=90/10(v/v),柱温为25℃,流速为1mL/min,检测波长为254nm。
(11)分析结果表明:样品中三氯联苯的浓度为0.1mg/L、六氯联苯的浓度为0.1mg/L。
实施例4
(1)称取70mg磁性颗粒并置于吸附萃取室内;
(2)使用热熔胶将PTFE微孔滤膜粘在搅拌室与吸附萃取室中间;
(3)再向该装置内加入50mL含有未知浓度三氯联苯和六氯联苯的样品溶液;
(4)向搅拌室内放置一个直径为1.5cm的搅拌子;
(5)将该装置置于磁力搅拌器上搅拌1小时;
(6)将装置从磁力搅拌器上取下后静置一分钟,后使用磁铁将磁性颗粒吸附在吸附萃取室内,然后除去水相;
(7)向吸附萃取室内加入2mL正己烷,超声解吸15分钟;
(8)解吸完成后,取0.5mL液体于一圆底烧瓶中,用氮气将烧瓶内正己烷吹干,后加入0.5mL色谱甲醇,超声处理两分钟,使多氯联苯溶解到色谱甲醇中;
(9)使用高效液相色谱分析上清液;
(10)液相色谱条件:采用C18柱,流动相为乙腈/水=90/10(v/v),柱温为25℃,流速为1mL/min,检测波长为254nm。
(11)分析结果表明:样品中三氯联苯的浓度为0.1mg/L、六氯联苯的浓度为0.1mg/L。
实施例5
(1)称取50mg磁性颗粒并置于吸附萃取室内;
(2)使用热熔胶将PTFE微孔滤膜粘在搅拌室与吸附萃取室中间;
(3)再向该装置内加入50mL含有未知浓度三氯联苯和六氯联苯的样品溶液;
(4)向搅拌室内放置一个直径为1.5cm的搅拌子;
(5)将该装置置于磁力搅拌器上搅拌1小时;
(6)将装置从磁力搅拌器上取下后静置一分钟,使用磁铁将磁性颗粒吸附在吸附萃取室内,然后除去水相;
(7)向吸附萃取室内加入2mL正己烷,超声解吸15分钟;
(8)解吸完成后,取0.5mL液体于一圆底烧瓶中,用氮气将烧瓶内正己烷吹干,后加入0.5mL色谱甲醇,超声处理两分钟,使多氯联苯溶解到色谱甲醇中;
(9)使用高效液相色谱分析上清液;
(10)液相色谱条件:采用C18柱,流动相为乙腈/水=90/10(v/v),柱温为25℃,流速为1mL/min,检测波长为254nm。
(11)分析结果表明:样品中三氯联苯的浓度为0.31mg/L、六氯联苯的浓度为0.30mg/L。
本说明书中各个实施例采用递进的方式描述,每个实施例重点说明的都是与其他实施例的不同之处,各个实施例之间相同相似部分互相参见即可。
对所公开的实施例的上述说明,使本领域专业技术人员能够实现或使用本发明。对这些实施例的多种修改对本领域的专业技术人员来说将是显而易见的,本文中所定义的一般原理可以在不脱离本发明的精神或范围的情况下,在其它实施例中实现。因此,本发明将不会被限制于本文所示的这些实施例,而是要符合与本文所公开的原理和新颖特点相一致的最宽的范围。
Claims (3)
1.一种适用于颗粒材料搅拌萃取的萃取装置,其特征在于,包括搅拌室、吸附萃取室和微孔滤膜;
所述搅拌室位于吸附萃取室的上方,微孔滤膜位于搅拌室和吸附萃取室的交接处;
所述微孔滤膜的直径大于搅拌室和吸附萃取室的交接处的中部瓶颈的直径;
所述搅拌室中放入搅拌子,搅拌子的长度小于搅拌室和吸附萃取室的交接处的中部瓶颈的直径;
所述吸附萃取室内放置磁性吸附剂。
2.权利要求1所述萃取装置的使用方法,其特征在于,包括以下步骤:
在吸附萃取室中加入磁性吸附剂;用热熔胶将微孔滤膜固定在搅拌室和吸附萃取室的交接处;向萃取装置中添加含有分析物的液体;在搅拌室中放入搅拌子,进行搅拌萃取。
3.根据权利要求2所述的使用方法,其特征在于,向萃取装置中添加含有分析物的液体时,利用洗耳球增大搅拌室压强,克服搅拌室与吸附萃取室的压强差,从而使液体顺利进入吸附萃取室与磁性吸附剂接触。
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Citations (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN104749277A (zh) * | 2015-03-26 | 2015-07-01 | 聊城大学 | 基于磁性竹炭分散基质固相萃取的多氯联苯检测方法 |
CN107875672A (zh) * | 2017-11-20 | 2018-04-06 | 福州大学 | 用于固体吸附材料的微萃取搅拌棒装置及其使用方法 |
CN108918221A (zh) * | 2018-07-12 | 2018-11-30 | 中国航发哈尔滨轴承有限公司 | 一种轴承钢中碳化物相低温电解萃取系统 |
CN109589808A (zh) * | 2018-12-27 | 2019-04-09 | 太原理工大学 | 一种碳基表面分子印迹二维复合膜的制备方法 |
CN110156090A (zh) * | 2019-06-28 | 2019-08-23 | 中国科学院合肥物质科学研究院 | 一种用于制备Fe3O4磁性纳米颗粒的流体合成制备装置及其控制方法 |
JP2019197035A (ja) * | 2018-05-11 | 2019-11-14 | 株式会社日立ハイテクノロジーズ | 撹拌装置、分析装置、分注方法 |
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CN104749277A (zh) * | 2015-03-26 | 2015-07-01 | 聊城大学 | 基于磁性竹炭分散基质固相萃取的多氯联苯检测方法 |
CN107875672A (zh) * | 2017-11-20 | 2018-04-06 | 福州大学 | 用于固体吸附材料的微萃取搅拌棒装置及其使用方法 |
JP2019197035A (ja) * | 2018-05-11 | 2019-11-14 | 株式会社日立ハイテクノロジーズ | 撹拌装置、分析装置、分注方法 |
CN108918221A (zh) * | 2018-07-12 | 2018-11-30 | 中国航发哈尔滨轴承有限公司 | 一种轴承钢中碳化物相低温电解萃取系统 |
CN109589808A (zh) * | 2018-12-27 | 2019-04-09 | 太原理工大学 | 一种碳基表面分子印迹二维复合膜的制备方法 |
CN110156090A (zh) * | 2019-06-28 | 2019-08-23 | 中国科学院合肥物质科学研究院 | 一种用于制备Fe3O4磁性纳米颗粒的流体合成制备装置及其控制方法 |
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