聚合物整体柱用于在线固相微萃取吸附环境污染物
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摘要
高效液相色谱法(HPLC)已广泛用于有机污染物的分析中。其中,样品前处理是富集分析物的重要过程。固相微萃取(SPME)是一种简单快速的前处理技术,用于从基质中分离和富集分析物。与常规萃取技术相比,固相微萃取溶剂用量少,可与高效液相色谱方便联用。
整体柱作为固相微萃取吸附剂,具有制备容易,柱压低,传质快等优点。通过改变单体和其相对比例,可控制孔的大小和结构。包括click反应在内的整体柱制备方法已有所应用。Huisgen1,3-偶极环加成反应是一个典型的click反应,自发现以来获得了广泛使用。在该反应中,铜(Ⅰ)作为催化剂,含炔基和叠氮基的化合物作为单体,生成1,2,3-三唑化合物。click反应常用于有机-无机杂化整体柱和聚合物整体柱的表面官能化。
在本实验中,以2,2′,7,7′-四乙炔基-9,9′-螺二芴(TES)和对二(6-叠氮己烷氧基)苯(BAB)作为单体,,Cu(PPh3)3Br为催化剂,应用click反应,合成了固相微萃取整体柱TES-BAB。该整体柱与高效液相色谱联用,测定了胺类、酚类、多环芳烃(PAHs)类、雌激素类的化合物。π-π堆积和尺寸效应是影响萃取的主要因素。
High-performance liquid chromatography (HPLC) method has been widely applied to analyze organic pollutants. In these analytical methods, sample pretreatment is an important process to enrichment the analyte. Solid-phase microextraction (SPME) is a simple and fast extraction technique, which has gained widespread acceptance for analyte matrix separation and preconcentration. Compared to the conventional solvent extraction techniques, it is a solvent-free technique and can be combined with HPLC.
Use of a monolith column as the sorbent in SPME has advantages including ease of preparation, low-pressure drop, and rapid mass transport. The pore size and structure of the column is controlled by changing the monomers and their relative proportions. To prepare a monolith column, various polymerization methods have been demonstrated, including the click reaction. The Huisgen1,3-dipolar cycloaddition reaction is an valuable click reaction, which has been implemented widely since its discovery. In this reaction, Cu(I) is used as catalyst, with alkynyl and azido as the active groups, to obtain1,2,3-triazole compounds. This type of click reaction is usually used for surface functionalization of a monolith column, in both the organic-inorganic hybrid monolith column and the polymer monolith column.
A polymer monolith column was prepared using click chemistry for on-line solid phase microextraction, using2,2',7,7'-tetraethynyl-9,9'-spirobifluorene(TES) and1,4-bis-(6-azidoalkoxy)-benzene(BAB) as monomers, and Cu(PPh3)3Br as the catalyst. The polymer monolith was used as on-line solid-phase microextraction adsorbent coupled to HPLC for determination of amines, phenols, polycyclic aromatic hydrocarbons (PAHs) and estrogens. The π-π stacking interaction and the effect of small size played dominant roles in the adsorption.
整体柱作为固相微萃取吸附剂,具有制备容易,柱压低,传质快等优点。通过改变单体和其相对比例,可控制孔的大小和结构。包括click反应在内的整体柱制备方法已有所应用。Huisgen1,3-偶极环加成反应是一个典型的click反应,自发现以来获得了广泛使用。在该反应中,铜(Ⅰ)作为催化剂,含炔基和叠氮基的化合物作为单体,生成1,2,3-三唑化合物。click反应常用于有机-无机杂化整体柱和聚合物整体柱的表面官能化。
在本实验中,以2,2′,7,7′-四乙炔基-9,9′-螺二芴(TES)和对二(6-叠氮己烷氧基)苯(BAB)作为单体,,Cu(PPh3)3Br为催化剂,应用click反应,合成了固相微萃取整体柱TES-BAB。该整体柱与高效液相色谱联用,测定了胺类、酚类、多环芳烃(PAHs)类、雌激素类的化合物。π-π堆积和尺寸效应是影响萃取的主要因素。
High-performance liquid chromatography (HPLC) method has been widely applied to analyze organic pollutants. In these analytical methods, sample pretreatment is an important process to enrichment the analyte. Solid-phase microextraction (SPME) is a simple and fast extraction technique, which has gained widespread acceptance for analyte matrix separation and preconcentration. Compared to the conventional solvent extraction techniques, it is a solvent-free technique and can be combined with HPLC.
Use of a monolith column as the sorbent in SPME has advantages including ease of preparation, low-pressure drop, and rapid mass transport. The pore size and structure of the column is controlled by changing the monomers and their relative proportions. To prepare a monolith column, various polymerization methods have been demonstrated, including the click reaction. The Huisgen1,3-dipolar cycloaddition reaction is an valuable click reaction, which has been implemented widely since its discovery. In this reaction, Cu(I) is used as catalyst, with alkynyl and azido as the active groups, to obtain1,2,3-triazole compounds. This type of click reaction is usually used for surface functionalization of a monolith column, in both the organic-inorganic hybrid monolith column and the polymer monolith column.
A polymer monolith column was prepared using click chemistry for on-line solid phase microextraction, using2,2',7,7'-tetraethynyl-9,9'-spirobifluorene(TES) and1,4-bis-(6-azidoalkoxy)-benzene(BAB) as monomers, and Cu(PPh3)3Br as the catalyst. The polymer monolith was used as on-line solid-phase microextraction adsorbent coupled to HPLC for determination of amines, phenols, polycyclic aromatic hydrocarbons (PAHs) and estrogens. The π-π stacking interaction and the effect of small size played dominant roles in the adsorption.
引文
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