CN106622183B - 固相微萃取纤维的制备方法及固相微萃取纤维 - Google Patents
固相微萃取纤维的制备方法及固相微萃取纤维 Download PDFInfo
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Abstract
本发明属于仪器分析技术领域,特别提供了一种新型固相微萃取纤维的制备方法及固相微萃取纤维。按照如下的工艺步骤制备:蚀刻‑有机溶剂超声清洗、烘干‑制备混合溶液A‑制备溶胶溶液B‑将不锈钢丝依次浸入混合溶液A和溶胶溶液B涂覆‑老化‑去除毛细管,最终得到制备好的新型固相微萃取纤维,具有涂层牢固、萃取效率高的优点。
Description
技术领域
本发明属于仪器分析技术领域,特别提供了一种固相微萃取纤维的制备方法及固相微萃取纤维。
背景技术
固相微萃取(Solod phase Micro-Extration SPME)是在固相萃取基础上发展起来的一种新的萃取分离技术,与液-液萃取和固相萃取相比,具有操作时间短,样品量小,无需萃取溶剂,适于分析挥发性与非挥发性物质,重现性好等优点。固相微萃取纤维是固相微萃取技术的核心部件,但是现有的固相微萃取纤维具有涂层容易脱落、萃取效率低等问题。
发明内容
为了解决上述技术问题,本发明提供了一种固相微萃取纤维的制备方法及固相微萃取纤维,通过该种方法制备的固相微萃取纤维具有涂层牢固、萃取效率高的优点。
本发明是这样实现的,根据本发明的一个方面,提供了一种固相微萃取纤维的制备方法,包括如下步骤:
1)将不锈钢丝放入等离子体发生器不锈钢网的负极上,导电棒接正极,电压设置在8-20kV,接通电源,在等离子体发生器中处理1min~150min,使不锈钢丝表面被蚀刻,增加表面积,增强其吸附能力,同时产生羟基,羰基等自由基;
2)将步骤1)中处理好的不锈钢丝用有机溶剂进行超声清洗、烘干;
3)取甲基丙烯酸,加入三甲氧基丙烷、三甲基丙烯酸酯、甲苯、偶氮二异丁腈,超声混匀、氮吹除氧后得预聚合混合溶液A;用微量进样器将上述混合液注入玻璃毛细管中待用;
4)取还原氧化石墨烯5mg于1.5mL的离心试管中,加入300μL二甲基甲酰胺,超声50-70min至均相,然后加入50μL氨基丙基三乙氧基硅烷及100μL甲基三甲氧基硅烷,超声5min混匀,最后加入95%的三氟乙酸水溶液,超声5min至均相,所得溶液为制备固相微萃取涂层的溶胶溶液B,用微量进样器将上述溶胶溶液注入玻璃毛细管中待用;
5)将处理过的不锈钢丝垂直浸入到配制好的混合溶液A中,缓慢抽动3-12下,使其涂抹均匀;将涂有混合溶液A的不锈钢丝垂直浸入到配制好的溶胶溶液B中,缓慢抽动3-12下,使其涂抹均匀;
6)将步骤5)中处理好的不锈钢丝在氮气保护下干燥24h,然后放入气相色谱仪进样口老化3h,温度由80℃上升到280℃;
7)去除毛细管,即得固相微萃取纤维。
进一步地,步骤1)中不锈钢丝在等离子体发生器中处理60-120min。
进一步地,步骤2)中所述有机溶剂为丙酮、乙醇中的一种。
进一步地,步骤3)中甲苯为溶剂,甲基丙烯酸浓度为0.01mmol/L、三甲氧基丙烷浓度为0.04mmol/L、三甲基丙烯酸酯浓度为0.04mmol/L 0.04、偶氮二异丁腈浓度为0.04mmol/L。
根据本发明的另外一个方面,还提供了一种按照上述的方法制备的固相微萃取纤维。
与现有技术相比,本发明的优点在于:通过本方法制备的固相微萃取纤维涂层牢固、具有更高的萃取效率。
具体实施方式
为了使本发明的目的、技术方案及优点更加清楚明白,下面结合实施例,对本发明进行进一步详细说明。应当理解,此处所描述的具体实施例仅仅用于解释本发明,并不用于限定本发明。
实施例1、
1)将不锈钢丝放入等离子体发生器不锈钢网的负极上,导电棒接正极,电压设置在8kV,接通电源,在等离子体发生器中处理1min,使不锈钢丝表面被蚀刻,增加表面积,增强其吸附能力,同时产生羟基,羰基等自由基;
2)将步骤1)中处理好的不锈钢丝用有机溶剂进行超声清洗、烘干;
3)取甲基丙烯酸0.01mmol,加入0.04mmol三甲氧基丙烷、0.04mmol三甲基丙烯酸酯0.04mmol、0.04mmol偶氮二异丁腈,溶于100ml甲苯中,超声混匀、氮吹除氧后得预聚合混合溶液A;用微量进样器将上述混合液注入玻璃毛细管中待用;
4)取还原氧化石墨烯5mg于1.5mL的离心试管中,加入300μL二甲基甲酰胺,超声50min至均相,然后加入50μL氨基丙基三乙氧基硅烷及100μL甲基三甲氧基硅烷,超声5min混匀,最后加入95%的三氟乙酸水溶液,超声5min至均相,所得溶液为制备固相微萃取涂层的溶胶溶液B,用微量进样器将上述溶胶溶液注入玻璃毛细管中待用;
5)将处理过的不锈钢丝垂直浸入到配制好的混合溶液A中,缓慢抽动3下,使其涂抹均匀;将涂有混合溶液A的不锈钢丝垂直浸入到配制好的溶胶溶液B中,缓慢抽动3下,使其涂抹均匀;
6)将步骤5)中处理好的不锈钢丝在氮气保护下干燥24h,然后放入气相色谱仪进样口老化3h,温度由80℃上升到280℃;
7)去除毛细管,即得固相微萃取纤维。
实施例2、
1)将不锈钢丝放入等离子体发生器不锈钢网的负极上,导电棒接正极,电压设置在20kV,接通电源,在等离子体发生器中处理150min,使不锈钢丝表面被蚀刻,增加表面积,增强其吸附能力,同时产生羟基,羰基等自由基;
2)将步骤1)中处理好的不锈钢丝用有机溶剂进行超声清洗、烘干;
3)取甲基丙烯酸0.01mmol,加入0.04mmol三甲氧基丙烷、0.04mmol三甲基丙烯酸酯0.04mmol、0.04mmol偶氮二异丁腈,溶于100ml甲苯中,超声混匀、氮吹除氧后得预聚合混合溶液A;用微量进样器将上述混合液注入玻璃毛细管中待用;
4)取还原氧化石墨烯5mg于1.5mL的离心试管中,加入300μL二甲基甲酰胺,超声70min至均相,然后加入50μL氨基丙基三乙氧基硅烷及100μL甲基三甲氧基硅烷,超声5min混匀,最后加入95%的三氟乙酸水溶液,超声5min至均相,所得溶液为制备固相微萃取涂层的溶胶溶液B,用微量进样器将上述溶胶溶液注入玻璃毛细管中待用;
5)将处理过的不锈钢丝垂直浸入到配制好的混合溶液A中,缓慢抽动12下,使其涂抹均匀;将涂有混合溶液A的不锈钢丝垂直浸入到配制好的溶胶溶液B中,缓慢抽动12下,使其涂抹均匀;
6)将步骤5)中处理好的不锈钢丝在氮气保护下干燥24h,然后放入气相色谱仪进样口老化3h,温度由80℃上升到280℃;
7)去除毛细管,即得固相微萃取纤维。
实施例3、
1)将不锈钢丝放入等离子体发生器不锈钢网的负极上,导电棒接正极,电压设置在14kV,接通电源,在等离子体发生器中处理75min,使不锈钢丝表面被蚀刻,增加表面积,增强其吸附能力,同时产生羟基,羰基等自由基;
2)将步骤1)中处理好的不锈钢丝用有机溶剂进行超声清洗、烘干;
3)取甲基丙烯酸0.01mmol,加入0.04mmol三甲氧基丙烷、0.04mmol三甲基丙烯酸酯0.04mmol、0.04mmol偶氮二异丁腈,溶于100ml甲苯中,超声混匀、氮吹除氧后得预聚合混合溶液A;用微量进样器将上述混合液注入玻璃毛细管中待用;
4)取还原氧化石墨烯5mg于1.5mL的离心试管中,加入300μL二甲基甲酰胺,超声60min至均相,然后加入50μL氨基丙基三乙氧基硅烷及100μL甲基三甲氧基硅烷,超声5min混匀,最后加入95%的三氟乙酸水溶液,超声5min至均相,所得溶液为制备固相微萃取涂层的溶胶溶液B,用微量进样器将上述溶胶溶液注入玻璃毛细管中待用;
5)将处理过的不锈钢丝垂直浸入到配制好的混合溶液A中,缓慢抽动7下,使其涂抹均匀;将涂有混合溶液A的不锈钢丝垂直浸入到配制好的溶胶溶液B中,缓慢抽动7下,使其涂抹均匀;
6)将步骤5)中处理好的不锈钢丝在氮气保护下干燥24h,然后放入气相色谱仪进样口老化3h,温度由80℃上升到280℃;
7)去除毛细管,即得固相微萃取纤维。
Claims (4)
1.固相微萃取纤维的制备方法,其特征在于,包括如下步骤:
1)将不锈钢丝放入等离子体发生器不锈钢网的负极上,导电棒接正极,电压设置在8-20kV,接通电源,在等离子体发生器中处理1~150min,使不锈钢丝表面被蚀刻,增加表面积,增强其吸附能力,同时产生羟基,羰基等自由基;
2)将步骤1)中处理好的不锈钢丝用有机溶剂进行超声清洗、烘干;
3)取0.01mmol甲基丙烯酸,加入0.04mmol三甲氧基丙烷、0.04mmol三甲基丙烯酸酯、100mL甲苯、0.04mmol偶氮二异丁腈,超声混匀、氮吹除氧后得预聚合混合溶液A;用微量进样器将上述混合液注入玻璃毛细管中待用,其中,甲苯为溶剂,甲基丙烯酸浓度为0.01mmol/L、三甲氧基丙烷浓度为0.04mmol/L、三甲基丙烯酸酯浓度为0.04mmol/L、偶氮二异丁腈浓度为0.04mmol/L;
4)取还原氧化石墨烯5mg于1.5mL的离心试管中,加入300μL二甲基甲酰胺,超声50-70min至均相,然后加入50μL氨基丙基三乙氧基硅烷及100μL甲基三甲氧基硅烷,超声5min混匀,最后加入95%的三氟乙酸水溶液,超声5min至均相,所得溶液为制备固相微萃取涂层的溶胶溶液B,用微量进样器将上述溶胶溶液注入玻璃毛细管中待用;
5)将处理过的不锈钢丝垂直浸入到配制好的混合溶液A中,缓慢抽动3-12下,使其涂抹均匀;将涂有混合溶液A的不锈钢丝垂直浸入到配制好的溶胶溶液B中,缓慢抽动3-12下,使其涂抹均匀;
6)将步骤5)中处理好的不锈钢丝在氮气保护下干燥24h,然后放入气相色谱仪进样口老化3h,温度由80℃上升到280℃;
7)去除毛细管,即得固相微萃取纤维。
2.按照权利要求1所述的固相微萃取纤维的制备方法,其特征在于,步骤1)中不锈钢丝在等离子体发生器中处理60-120min。
3.按照权利要求1所述的固相微萃取纤维的制备方法,其特征在于,步骤2)中所述有机溶剂为丙酮、乙醇中的一种。
4.一种按照权利要求1-3任一所述的方法制备的固相微萃取纤维。
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