CN106000327B - 一种富集微囊藻毒素的Fe3O4@SiO2@CPC磁性纳米材料的制备方法 - Google Patents

一种富集微囊藻毒素的Fe3O4@SiO2@CPC磁性纳米材料的制备方法 Download PDF

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CN106000327B
CN106000327B CN201610425151.0A CN201610425151A CN106000327B CN 106000327 B CN106000327 B CN 106000327B CN 201610425151 A CN201610425151 A CN 201610425151A CN 106000327 B CN106000327 B CN 106000327B
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CN106000327A (zh
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娄大伟
李秋颖
祝波
连丽丽
王希越
田媛媛
王润楠
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Jilin Institute of Chemical Technology
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Abstract

本发明提供了一种富集微囊藻毒素的Fe3O4@SiO2@CPC磁性纳米材料的制备方法，它以Fe3O4@SiO2为载体，与氯代十六烷基吡啶（CPC）、去离子水、无水乙醇和氨水混合，得到黑色均一的液体，进行机械搅拌并逐滴加入正硅酸乙酯（TEOS）制得功能化磁性纳米材料。本发明制备出的磁性纳米材料具有较高的超顺磁性、稳定的化学性质及良好的分散性等特点，可用于环境中微囊藻毒素MC‑LR、MC‑RR的富集。本发明方法简单，原料易得且成本低，在分析化学领域中有广阔的应用前景。

Description

一种富集微囊藻毒素的Fe3O4@SiO2@CPC磁性纳米材料的制备 方法
技术领域
本发明属于无机复合材料与技术领域，具体涉及一种新型磁性纳米材料的制备，此材料可应用于环境中痕量微囊藻毒素（MC-LR，MC-RR）的富集。
背景技术
微囊藻毒素(Microcystin，MC)是一类具有生物活性的环状七肽化合物，是一种分布最广泛的肝毒素之一。随着中国水体的富营养化程度逐渐加剧，蓝藻水华和赤潮的发生逐渐增加。80%的蓝藻水华水中都可以检测出次生代谢产物-微囊藻毒素，它对水体环境和人群健康的危害已成为全球关注的重大环境问题之一。由此可见，对水环境中微囊藻毒素的检测和控制变得越来越重要。
磁性固相萃取技术是在含有目标分析物的溶液中加入磁性吸附材料，使目标分析物被吸附，再通过外加磁场使目标分析物和样品基质快速分离。将磁性固相萃取引入环境样品前处理技术，磁性吸附材料不仅可以直接在环境介质中进行富集和快速分离，而且还避免了传统固相萃取填充柱中高背压、柱堵塞和吸附剂用量大等问题。通过对磁性纳米颗粒表面进行修饰，不仅能够提高磁性粒子对目标分析物的选择性，而且可以保护磁性颗粒在环境基质中不被氧化，这使得对目标分析物的分离富集变得更加高效、快速、便捷。
本发明以氯代十六烷基吡啶为模版制备Fe3O4@SiO2磁性纳米粒子，经修饰后的磁性纳米材料具有稳定的化学性质和高选择性等优点，并在富集环境水样中的MC-LR、MC-RR显示了独特的优势。
发明内容
本发明提供了一种用于富集微囊藻毒素MC-LR、MC-RR的功能化磁性纳米粒子的制备方法。具体制备方法如下：
（1）将Fe3O4@SiO2加入到含有氯代十六烷基吡啶(CPC)， 80 ml去离子水，60 ml无水乙醇，1 ml 25%氨水的混合体系中，并将其混合均匀，得到黑色均一液体；
（2）将上述液体转移到250 ml三口烧瓶中，使用机械搅拌器进行搅拌，转速为200rpm，逐滴加入正硅酸乙酯（TEOS），连续搅拌6~8 h;
（3）将得到的磁性纳米材料用去离子水和无水乙醇清洗，在真空干燥箱中60 °C烘干2 h。
附图说明
图1磁性纳米粒子透射电镜（TEM）图。
图2吸附剂加入量对MC-LR、MC-RR的吸附结果影响。
具体实施方式
磁性纳米粒子制备实施例：
将制备的Fe3O4@SiO2以及氯代十六烷基吡啶（CPC）、去离子水、无水乙醇和25%氨水混合得到黑色均一液体，将上述液体转移到250 ml三口烧瓶中，用机械搅拌器以200 rmp的转速搅拌，温度控制在20°C，并逐滴加入正硅酸乙酯（TEOS），搅拌6 h。用去离子水和无水乙醇各清洗三次，在60 °C真空干燥箱中烘干2 h即得到Fe3O4@SiO2@ CPC粉末。
磁性纳米粒子的应用实例:
分别称取2 mg、4 mg、6 mg、8 mg、10 mg、12 mg的Fe3O4@SiO2@ CPC磁性纳米粒子分别放入含有MC-LR、MC-RR的100 ml混合液中，该溶液中MC-LR、MC-RR的浓度均为1 ug/L，涡旋震荡10 min，对磁性纳米粒子进行回收，用800 μl体积比为1：3的乙腈和水（含0.2%的三氟乙酸，v/v）洗脱液对粒子进行洗脱，超声10 min，回收洗脱液，用氮气将其吹干，再加入200 μl的超纯水定容，利用液相色谱检测。

Claims (2)

1.一种富集微囊藻毒素的Fe3O4@SiO2@CPC磁性纳米材料的制备方法，其特征在于：以Fe3O4@SiO2为载体，按照质量比Fe3O4@SiO2：氯代十六烷基吡啶为1:1的比例取Fe3O4@SiO2和氯代十六烷基吡啶加入到80ml去离子水，60ml无水乙醇，1ml 25％氨水的混合体系中，并将其混合均匀，得到黑色均一液体；将上述液体转移到250ml三口烧瓶中，使用机械搅拌器进行搅拌，并逐滴加入正硅酸乙酯，正硅酸乙酯与氯代十六烷基吡啶质量比为4:1，连续搅拌6～8h，机械搅拌器的转速为200rpm，机械搅拌的温度为20℃～30℃；将得到的磁性纳米材料用去离子水和无水乙醇清洗，在60℃真空干燥箱中烘干2h。
2.按照权利要求1所述的制备方法，其特征在于：氯代十六烷基吡啶的质量为0.1g。
CN201610425151.0A 2016-06-16 2016-06-16 一种富集微囊藻毒素的Fe3O4@SiO2@CPC磁性纳米材料的制备方法 Active CN106000327B (zh)

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CN104128160A (zh) * 2014-08-18 2014-11-05 吉林化工学院 一种用于去除微囊藻毒素mc-lr的磁性纳米粒子的制备方法
CN104892869A (zh) * 2015-06-23 2015-09-09 嘉兴学院 用于检测微囊藻毒素的磁性聚合离子液体及其制备方法和应用

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CN104128160A (zh) * 2014-08-18 2014-11-05 吉林化工学院 一种用于去除微囊藻毒素mc-lr的磁性纳米粒子的制备方法
CN104892869A (zh) * 2015-06-23 2015-09-09 嘉兴学院 用于检测微囊藻毒素的磁性聚合离子液体及其制备方法和应用

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