CN107413317B - 壳聚糖改性gma/maa聚合物吸附剂及其方法和应用 - Google Patents
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Abstract
本发明涉及壳聚糖改性GMA/MAA聚合物吸附剂及其方法和应用,所述方法如下:(1)GMA/MAA聚合物吸附剂:取体积比为4:14‑15的甲基丙烯酸和甲基丙烯酸缩水甘油酯与乙二醇二甲基丙烯酸脂、十二烷醇、环己醇、偶氮二异丁腈超声混匀,将聚合液于50‑60℃反应,然后用甲醇洗涤,烘干得到GMA/MAA聚合物吸附剂;(2)壳聚糖改性GMA/MAA聚合物吸附剂:向蒸馏水中加入GMA/MAA聚合物吸附剂、冰醋酸及壳聚糖,超声处理,于60‑70℃下进行反应,反应结束后加入甲醇洗涤,离心,去除上清液,烘干得到壳聚糖改性GMA/MAA聚合物吸附剂。制备的壳聚糖改性聚GMA/MAA可用于固相萃取检测洛美沙星。
Description
技术领域
本发明属于聚合物微球技术领域,具体涉及一种壳聚糖改性GMA/MAA聚合物吸附剂及其方法和应用。
背景技术
固相萃取(SPE)是从上世纪八十年代发展起来的一项样品前处理技术。SPE是利用固体吸附剂将液体样品中的目标化合物吸附,与样品基体和干扰化合物分离,然后再用洗脱液进行洗脱,从而达到分离目标化合物的目的。其具有简单、快速和简化了样品预处理操作步骤,缩短了预处理时间;并且可选择不同类型的吸附剂和有机溶剂处理各种不同类型的有机污染物。此外,SPE易于与其他仪器联用,实现自动化在线分析等优点,已被广泛应用。
壳聚糖是一种天然的阳离子高分子多糖,它来源丰富、无毒、无污染、生物相容性好及可降解性强,已广泛应用于食品、环保等诸多领域。因分子中有游离氨基,因此在酸性条件下,带有阳离子电荷的高分子聚合物可以和阴离子高分子聚合物形成复合物。壳聚糖分子中氨基和羟基具有孤对电子及空轨道,因此具有良好的吸附能力。另外,氨基质子化形成的阳离子也可与阴离子发生静电结合,因此壳聚糖可以吸附结合许多无机酸、酸性化合物和有机酸,甚至也可以吸附结合两性化合物。壳聚糖具有亲水性、生物相容性、可降解等特点,此外壳聚糖及其衍生物的分子链上存在着游离的氨基和羟基,因此可用于吸附检测食品以及人体组织液中金属离子、有机小分子等物质,具有广泛的应用前景。
发明内容
本发明主要提供了一种壳聚糖改性GMA/MAA聚合物吸附剂及其方法和应用,制备的壳聚糖改性聚GMA/MAA可用于固相萃取检测洛美沙星。其技术方案如下:
一种壳聚糖改性GMA/MAA聚合物吸附剂的方法,包括以下步骤:
(1)GMA/MAA聚合物吸附剂的制备
取体积比为4:14-15的甲基丙烯酸和甲基丙烯酸缩水甘油酯与乙二醇二甲基丙烯酸脂、十二烷醇、环己醇、偶氮二异丁腈超声混匀,将聚合液于50-60℃下反应,然后用甲醇洗涤,烘干得到GMA/MAA聚合物吸附剂;
(2)壳聚糖改性GMA/MAA聚合物吸附剂
向蒸馏水中加入GMA/MAA聚合物吸附剂、冰醋酸及壳聚糖,超声处理,并于60-70℃下进行反应,反应结束后加入甲醇洗涤,离心,去除上清液,烘干得到壳聚糖改性GMA/MAA聚合物吸附剂。
优选的,乙二醇二甲基丙烯酸脂与甲基丙烯酸的体积比为3-3.2:1,十二烷醇与甲基丙烯酸的体积比为2.9-3.2:1,环己醇与甲基丙烯酸的体积比为24-26:1。
一种壳聚糖改性GMA/MAA聚合物吸附剂,其由上述方法制备而成。
上述制备的壳聚糖改性GMA/MAA聚合物吸附剂可以用于萃取洛美沙星。
一种壳聚糖改性GMA/MAA聚合物吸附剂萃取检测洛美沙星的方法,包括以下步骤:
(1)称取壳聚糖改性GMA/MAA聚合物吸附剂于容器中,加入甲醇进行超声处理,然后离心去除上清液;
(2)将待测的洛美沙星溶液加入容器中,超声处理,然后离心去除上清液;
(3)向容器中加入蒸馏水,超声处理,然后离心去除上清液;
(4)向容器中加入甲醇水溶液,超声处理,离心取上清液,在波长276nm处测定吸光度。
优选的,所述甲醇水溶液中甲醇的体积含量为20%。
优选的,在进行检测待测溶液的吸光度之前,配制洛美沙星的不同标准浓度,建立洛美沙星浓度与吸光度标准曲线,通过待测溶液的吸光度在标准曲线上找到相应浓度即可。
采用上述方案,本发明具有以下优点:
壳聚糖具有亲水性、生物相容性、可降解性等特点,此外壳聚糖及其衍生物的分子链上存在着游离的氨基和羟基,因此可用于吸附检测食品以及人体组织液中金属离子、有机小分子等物质,壳聚糖改性聚GMA/MAA用于固相萃取检测洛美沙星,以固相萃取法作为前处理方法,在波长276nm处对洛美沙星含量进行测定。该方法制备过程简单、操作简便。此外,该复合材料表面含有利于洛美沙星吸附的特征性基团,能提高目标物的富集能力。
附图说明
图1为GMA/MAA聚合物吸附剂的扫描电镜图;
图2为GMA/MAA聚合物吸附剂的红外光谱图其中:(a)壳聚糖改性GMA/MAA聚合物吸附剂;(b)聚GMA/MAA聚合物;
图3为洛美沙星紫外光谱图;
图4为洛美沙星浓度与吸光度标准曲线图;
具体实施方式
以下实施例中的实验方法如无特殊规定,均为常规方法,所涉及的实验试剂及材料如无特殊规定均为常规生化试剂和材料。
实施例1
一、GMA/MAA聚合物吸附剂制备
GMA/MAA聚合物吸附剂的制备步骤如下:取40μL甲基丙烯酸(MAA)、145μL甲基丙烯酸缩水甘油酯(GMA)、125μL乙二醇二甲基丙烯酸脂、123μL十二烷醇、1mL环己醇、0.004g偶氮二异丁腈放入离心管中,超声30min混匀。随后将聚合液放在55℃下反应24h。反应结束后用甲醇洗涤,除去未反应的单体和交联剂。最后将复合物烘干,备用。
制备的GMA/MAA聚合物吸附剂电镜下的扫描图如图1所示,红外光谱图如图2所示,其中聚GMA/MAA聚合物为b所示,壳聚糖改性GMA/MAA聚合物吸附剂为a所示。
二、壳聚糖改性GMA/MAA聚合物的制备
取一定量的聚GMA/MAA聚合物,加入1mL的蒸馏水、10μL的冰醋酸、0.01g壳聚糖,超声60min,在65℃条件下,反应4h;反应结束后加入甲醇反复洗涤、离心,去除上清液,在55℃下烘干、备用。
三、洛美沙星的萃取和检测
(1)洛美沙星紫外光谱图如图3所示,配制洛美沙星的不同标准浓度,建立洛美沙星浓度与吸光度标准曲线,如图4所示;
(2)称取0.02g壳聚糖改性GMA/MAA聚合物吸附剂放入离心管中,加入1mL的甲醇,超声3min,离心去除上清液;
(3)将待测的洛美沙星溶液加入容器中,超声20min,离心去除上清液;
(4)向容器中加入1mL的蒸馏水,超声3min,离心去除上清液;
(5)加入含有20%的甲醇水溶液,超声10min,离心取上清液,在波长为276nm处测定吸光度。
实施例2
一、GMA/MAA聚合物吸附剂制备
GMA/MAA聚合物吸附剂的制备步骤如下:取40μL甲基丙烯酸(MAA)、150μL甲基丙烯酸缩水甘油酯(GMA)、128μL乙二醇二甲基丙烯酸脂、128μL十二烷醇、1mL环己醇、0.004g偶氮二异丁腈放入离心管中,超声30min混匀。随后将聚合液放在60℃下反应24h。反应结束后用甲醇洗涤,除去未反应的单体和交联剂。最后将复合物烘干,备用。
二、壳聚糖改性GMA/MAA聚合物的制备
取一定量的聚GMA/MAA聚合物,加入1mL的蒸馏水、10μL的冰醋酸、0.01g壳聚糖,超声60min,在70℃条件下,反应4h;反应结束后加入甲醇反复洗涤、离心,去除上清液,在55℃下烘干、备用。
三、洛美沙星的萃取和检测
(1)配制洛美沙星的不同标准浓度,建立洛美沙星浓度与吸光度标准曲线;
(2)称取0.02g壳聚糖改性GMA/MAA聚合物吸附剂放入离心管中,加入1mL的甲醇,超声3min,离心去除上清液;
(3)将待测的洛美沙星溶液加入容器中,超声20min,离心去除上清液;
(4)向容器中加入1mL的蒸馏水,超声3min,离心去除上清液;
(5)加入含有20%的甲醇水溶液,超声10min,离心取上清液,在波长为276nm处测定吸光度。
对本领域的技术人员来说,可根据以上描述的技术方案以及构思,做出其它各种相应的改变以及形变,而所有的这些改变以及形变都应该属于本发明权利要求的保护范围之内。
Claims (7)
1.一种壳聚糖改性GMA/MAA聚合物吸附剂的制备方法,其特征在于:包括以下步骤:
(1)GMA/MAA聚合物吸附剂的制备
取体积比为4:14-15的甲基丙烯酸(MAA)和甲基丙烯酸缩水甘油酯(GMA)与乙二醇二甲基丙烯酸酯、十二烷醇、环己醇、偶氮二异丁腈超声混匀,将聚合液于50-60℃下反应,然后用甲醇洗涤,烘干得到GMA/MAA聚合物吸附剂;
(2)壳聚糖改性GMA/MAA聚合物吸附剂
向蒸馏水中加入GMA/MAA聚合物吸附剂、冰醋酸及壳聚糖,超声处理,并于60-70℃下进行反应,反应结束后加入甲醇洗涤,离心,去除上清液,烘干得到壳聚糖改性GMA/MAA聚合物吸附剂。
2.根据权利要求1所述的壳聚糖改性GMA/MAA聚合物吸附剂的制备方法,其特征在于:乙二醇二甲基丙烯酸酯与甲基丙烯酸的体积比为3-3.2:1,十二烷醇与甲基丙烯酸的体积比为2.9-3.2:1,环己醇与甲基丙烯酸的体积比为24-26:1。
3.一种壳聚糖改性GMA/MAA聚合物吸附剂,其由权利要求1所述的方法制备而成。
4.权利要求3所述的壳聚糖改性GMA/MAA聚合物吸附剂在萃取洛美沙星方面的应用。
5.一种权利要求3所述的壳聚糖改性GMA/MAA聚合物吸附剂萃取检测洛美沙星的方法,其特征在于:包括以下步骤:
(1)称取壳聚糖改性GMA/MAA聚合物吸附剂于容器中,加入甲醇进行超声处理,然后离心去除上清液;
(2)将待测的洛美沙星溶液加入容器中,超声处理,然后离心去除上清液;
(3)向容器中加入蒸馏水,超声处理,然后离心去除上清液;
(4)向容器中加入甲醇水溶液,超声处理,离心取上清液,在波长276nm处测定吸光度。
6.根据权利要求5所述的壳聚糖改性GMA/MAA聚合物吸附剂萃取检测洛美沙星的方法,其特征在于:所述甲醇水溶液中甲醇的体积含量为20%。
7.根据权利要求5所述的壳聚糖改性GMA/MAA聚合物吸附剂萃取检测洛美沙星的方法,其特征在于:在进行检测待测溶液的吸光度之前,配制洛美沙星的不同标准浓度,建立洛美沙星浓度与吸光度标准曲线,通过待测溶液的吸光度在标准曲线上找到相应浓度即可。
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