CN108034055B - 一种共价有机骨架固相微萃取纤维及其制备方法 - Google Patents

一种共价有机骨架固相微萃取纤维及其制备方法 Download PDF

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CN108034055B
CN108034055B CN201711470362.7A CN201711470362A CN108034055B CN 108034055 B CN108034055 B CN 108034055B CN 201711470362 A CN201711470362 A CN 201711470362A CN 108034055 B CN108034055 B CN 108034055B
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牛佳佳
范黎
陈连芳
李栋
张勍
马明
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Zhengzhou Tobacco Research Institute of CNTC
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Abstract

本发明公开了一种共价有机骨架固相微萃取纤维及其制备方法，该固相微萃取纤维选用不锈钢丝、石英丝作为载体，以三(4‑溴苯基)胺为原料制备共价有机骨架材料（简称JUC‑Z2）；以硅氧烷和羟基封端的硅氧烷为凝胶原料，后加入JUC‑Z2粉末涡旋分散，将处理过的不锈钢丝插入混合溶液浸渍涂覆，后置于烘箱高温下固化，重复该浸渍涂覆及烘箱固化过程5～10次得到固相微萃取纤维。该纤维具有稳定性好、吸附性能优异、耐湿性好以及使用寿命长等特点，可用于食品、环境、卷烟烟气等实际样品中痕量组分的分析。

Description

一种共价有机骨架固相微萃取纤维及其制备方法
技术领域
本发明涉及固相微萃取纤维制备技术，具体地说是一种共价有机骨架固相微萃取纤维及其制备方法，属于分析化学领域。
背景技术
固相微萃取（SPME）是一种新兴的样品前处理技术，它是利用涂覆在纤维上的涂层材料将样品中的目标吸附、分离和富集。由于SPME技术是集萃取、浓缩、解吸和进样于一体的样品预处理技术，具有使用方便、快捷、无需有机溶剂、灵敏、价廉等优点，已被广泛用于样品预处理。
SPME技术的核心在于纤维上的涂层材料，目前商品化的涂层有聚二甲基硅氧烷（PDMS）、聚丙烯酸（PA）、聚乙二醇（CW）和碳分子筛（CAR）等不同厚度的单一、混合或共聚物涂层。对于特定的样品，选用合适的涂层非常重要。目前商品化的涂层种类有限，而且价格昂贵，适用温度较低，所以制备适用范围广、廉价的涂层显得非常重要。另一方面，现有技术制备的萃取纤维难以在超过300℃的条件下使用，且对于目标物的吸附能力有待进一步提高。
共价-有机骨架（Covalent Organic Framework, COF）是以轻元素H、B、O、C、Si等以共价键连接聚合构建的有序多孔材料。多样可调的孔道结构，良好的吸附性能，优异的热稳定性使其成为SPME 涂层的理想候选，但粉末状的COFs材料难以直接利用，其与不锈钢丝、石英等载体之间的结合牢固性是影响所制备纤维寿命的关键所在。因此，利用COFs材料的良好特性，发展一种合适的制备方法将高性能的COFs材料牢固地结合在载体纤维，制备出富集能力强、稳定性好、使用寿命长的新型COFs涂层SPME纤维是非常必要的。
发明内容：
本发明目的旨在提供一种富集效率高、稳定性好、使用寿命长的新型SPME纤维。
本发明的目的是通过以下技术方案来实现的：
一种共价有机骨架固相微萃取纤维，包括载体纤维和附着在其表面的涂层，其中：载体纤维为长度0.5～5 cm的不锈钢丝或石英丝，一端（约0.3～4.5 cm）涂覆有涂层材料，该涂层材料为JUC-Z2与凝胶所形成的复合材料（简称JUC-Z2/Gel）。具体步骤如下：
1）JUC-Z2的制备
双(1,5-环辛二烯)镍(0)、2,2'-联吡啶、1,5-环辛二烯按照1:1:1.1的摩尔比加入至80 mL无水二甲基甲酰胺（DMF）中，80 ℃下加热1 h，后加入0.5～1.0 mmol三(4-溴苯基)胺80 ℃下过夜反应。冷却至室温，加入36%（质量比）的盐酸使溶液变为绿色。过滤后，依次用水、乙醇和三氯甲烷冲洗，真空干燥后研磨成细微颗粒；
2）载体纤维的处理
对于不锈钢丝，依次用丙酮、甲醇和蒸馏水超声处理不锈钢丝，后在空气中干燥后，将钢丝一头置于40%（质量比）氢氟酸溶液中5～10 min，后用蒸馏水冲洗，室温下干燥待用；对于石英丝，将一头置1 mol/L氢氧化钠溶液中10～60 min，后用蒸馏水冲洗，室温下干燥待用；
3）固相微萃取纤维制备
将制备的JUC-Z2粉末0.05～2 g、硅氧烷300 μL和端羟基聚硅氧烷90 mg加入至试管中混合均匀，后加入150 μL三氟乙酸涡旋5 min；将处理过的载体纤维插入混合溶液浸渍涂覆，后置于烘箱180～230 ℃下固化20～30 min，重复该浸渍涂覆及烘箱固化过程5～10次得到固相微萃取纤维。
所述硅氧烷为二甲基二甲氧基硅烷、甲基三甲氧基硅烷、四甲氧基硅烷。
本发明提供了一种简单、快速、高效的SPME纤维制备方法，具有如下优势：1）采用凝胶与JUC-Z2复合的策略，一步制备JUC-Z2/Gel复合材料，同时完成复合材料在钢丝表面成膜；2）利用JUC-Z2高的比表面积、规整的孔道等结构特征，从而使JUC-Z2/Gel复合材料涂层具备对有机小分子良好的富集性能；3）JUC-Z2和凝胶两种材料均具有较好的高温稳定性、水和空气稳定性，因此所制备的JUC-Z2/Gel复合材料SPME纤维具备高的稳定性和使用寿命，同时可以应用于高湿性样品的检测中。
附图说明
图1：本发明实例1所制备SPME纤维扫描电镜图；
图2：本发明实例2所制备SPME纤维扫描电镜图。
具体实施方式
本发明以下结合实例做进一步描述，但并不是限制本发明。
实施例1：
1. JUC-Z2的制备
根据权利要求书中限定的摩尔比，称取双(1,5-环辛二烯)镍(0)、2,2'-联吡啶、1,5-环辛二烯2.9 mmol、2.9 mmol、3.2 mmol加入至80 mL无水DMF中，80 ℃下加热1 h，后加入0.8 mmol三(4-溴苯基)胺80 ℃下过夜反应。冷却至室温，加入36%的浓盐酸使溶液变为绿色。过滤后，依次用水、乙醇和三氯甲烷冲洗，真空干燥后研磨成细微颗粒；
2. 不锈钢丝处理
依次用丙酮、甲醇和蒸馏水超声处理不锈钢丝，后在空气中干燥后，将钢丝一头（约3cm）置于40%氢氟酸溶液中5 min，后用蒸馏水冲洗，室温下干燥待用。
3. SPME纤维制备
将制备的JUC-Z2粉末0.5 g、二甲基二甲氧基硅烷300 μL和端羟基聚硅氧烷90 mg加入至试管中混合均匀，后加入150 μL三氟乙酸涡旋5 min；将处理过的载体纤维插入混合溶液浸渍涂覆，后置于烘箱200 ℃下固化30 min，重复该浸渍涂覆及烘箱固化过程6次得到固相微萃取纤维。
实施例2：
1. JUC-Z2的制备
根据权利要求书中限定的摩尔比，称取双(1,5-环辛二烯)镍(0)、2,2'-联吡啶、1,5-环辛二烯2 mmol、2 mmol、2.2 mmol加入至80 mL无水DMF中，80 ℃下加热1 h，后加入0.6mmol三(4-溴苯基)胺80 ℃下过夜反应。冷却至室温，加入36%的浓盐酸使溶液变为绿色。过滤后，依次用水、乙醇和三氯甲烷冲洗，真空干燥后研磨成细微颗粒；
2. 石英丝处理
将石英丝一头置于1 mol/L氢氧化钠溶液中60 min后用蒸馏水冲洗，室温下干燥待用；
3. SPME纤维制备
将制备的JUC-Z2粉末0.8 g、甲基三甲氧基硅烷300 μL和端羟基聚硅氧烷90 mg加入至试管中混合均匀，后加入150 μL三氟乙酸涡旋5 min；将处理过的载体纤维插入混合溶液浸渍涂覆，后置于烘箱220 ℃下固化30 min，重复该浸渍涂覆及烘箱固化过程4次得到固相微萃取纤维。

Claims (2)

1.一种共价有机骨架固相微萃取纤维的制备方法，包括纤维载体和附着在其表面的涂层，其特征在于：载体纤维为长度0.5～5 cm的不锈钢丝或石英丝，其中一端涂覆有涂层材料，该涂层材料为JUC-Z2与聚甲氧基硅氧烷所形成的复合材料，简称JUC-Z2/gel；
具体方法如下：
1）JUC-Z2的制备
双(1,5-环辛二烯)镍(0)、2,2'-联吡啶、1,5-环辛二烯按照1:1:1.1的摩尔比加入至80mL无水二甲基甲酰胺DMF中，80 ℃下加热1 h，后加入0.5～1.0 mmol三(4-溴苯基)胺80 ℃下过夜反应；冷却至室温，加入36%盐酸使溶液变为绿色；过滤后，依次用水、乙醇和三氯甲烷冲洗，真空干燥后研磨成细微颗粒；
2）载体纤维的处理
对于不锈钢丝，依次用丙酮、甲醇和蒸馏水超声处理不锈钢丝，后在空气中干燥后，将钢丝一头置于40%氢氟酸溶液中5～10 min，后用蒸馏水冲洗，室温下干燥待用；对于石英丝，将一头置1 mol/L氢氧化钠溶液中10～60 min，后用蒸馏水冲洗，室温下干燥待用；
3）固相微萃取纤维制备
将制备的JUC-Z2粉末0.05～2 g、硅氧烷300 μL和端羟基聚硅氧烷90 mg加入至试管中混合均匀，后加入150 μL三氟乙酸，涡旋5 min；将处理过的载体纤维插入混合溶液浸渍涂覆，后置于烘箱180～230 ℃下固化20～30 min，重复该浸渍涂覆及烘箱固化过程5～10次得到固相微萃取纤维。
2.如权利要求1所述的共价有机骨架固相微萃取纤维的制备方法，其特征在于：所述硅氧烷为二甲基二甲氧基硅烷、甲基三甲氧基硅烷、四甲氧基硅烷。
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CN109621911A (zh) * 2019-01-31 2019-04-16 烟台大学 一种多孔有机骨架涂层的spme萃取纤维及其制备方法
CN110904685B (zh) * 2019-11-29 2020-07-28 中国科学院兰州化学物理研究所 一种二维共价有机框架改性柔性纤维织物及其制备方法
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