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离子液体调控的溶胶-凝胶整体柱用于水样和头发样品中农药残留的中空纤维固相微萃取。

Ionic liquid mediated sol-gel sorbents for hollow fiber solid-phase microextraction of pesticide residues in water and hair samples.

机构信息

Department of Chemistry, Faculty of Sciences, Birjand University, Birjand, Iran.

出版信息

J Chromatogr A. 2011 Nov 18;1218(46):8313-21. doi: 10.1016/j.chroma.2011.09.058. Epub 2011 Sep 29.

Abstract

An ionic liquid mediated sol-gel sorbents for hollow fiber solid-phase microextraction (HF-SPME) was developed for extraction of the pesticides: diazinon, fenitrothion, malathion, fenvalerate, phosalone and tridemorph from human hair and water samples. The analytes were subsequently analyzed with high performance liquid chromatography and diode array detection (HPLC-DAD). Preliminary experiments were carried out in order to study experimental conditions for pesticides' extraction from spiked hair and water samples with HF-SPME using hollow fiber-supported ionic liquid mediated sol-gel sorbent. The sol-gel nanocomposites were reinforced with nanoparticles such as carboxylic functionalized multi-walled carbon nanotubes (COOH-MWCNTs), amino functionalized multi-walled carbon nanotubes (NH(2)-MWCNTs), nano SiO(2), nano TiO(2) and nano MgO comparatively to promote extraction efficiency. In this device, the innovative solid sorbents were developed by the sol-gel method via the reaction of tetraethylorthosilicate (TEOS) with 2-amino-2-hydroxymethyl-propane-1,3-diol (TRIS). In the basic condition (pH 10-11), the gel growth process in the presence of ionic liquid and nanoparticles was initiated. Then, the sol was injected into a polypropylene hollow fiber segment for in situ gelation process. Parameters affecting the efficiency of HF-SPME were thoroughly investigated. Linearity was observed over a range of 0.01-25,000 ng/mL with detection limits between 0.004 and 0.095 ng/mL for the pesticides in the aqueous matrices and 0.003-0.080 ng/mL in the hair matrices. The relative recoveries in the real samples ranged from 82.0% to 94.0% for the pesticides store seller's hair and the work researchers' hair. Results are showing the great possibilities of HF-SPME-HPLC-PDA for analysis of pesticides in biological and environmental samples.

摘要

一种离子液体介导的溶胶-凝胶吸附剂被开发用于空心纤维固相微萃取(HF-SPME),用于从人发和水样中提取农药:二嗪农、杀螟硫磷、马拉硫磷、氰戊菊酯、磷丹和三唑酮。分析物随后用高效液相色谱和二极管阵列检测(HPLC-DAD)进行分析。进行了初步实验,以研究使用空心纤维支撑的离子液体介导的溶胶-凝胶吸附剂从加标头发和水样中萃取农药的实验条件。溶胶-凝胶纳米复合材料通过四乙氧基硅烷(TEOS)与 2-氨基-2-羟甲基-1,3-丙二醇(TRIS)的反应,用纳米粒子如羧酸功能化多壁碳纳米管(COOH-MWCNTs)、氨基功能化多壁碳纳米管(NH(2)-MWCNTs)、纳米 SiO(2)、纳米 TiO(2) 和纳米 MgO 进行增强,以提高萃取效率。在该装置中,通过溶胶-凝胶法在离子液体和纳米粒子的存在下,通过溶胶-凝胶法开发了创新的固态吸附剂。然后,将溶胶注入到聚丙烯空心纤维段中进行原位凝胶化过程。详细研究了影响 HF-SPME 效率的参数。在碱性条件下(pH 10-11),在离子液体和纳米粒子的存在下开始凝胶生长过程。然后,将溶胶注入到聚丙烯空心纤维段中进行原位凝胶化过程。详细研究了影响 HF-SPME 效率的参数。在碱性条件下(pH 10-11),在离子液体和纳米粒子的存在下开始凝胶生长过程。然后,将溶胶注入到聚丙烯空心纤维段中进行原位凝胶化过程。详细研究了影响 HF-SPME 效率的参数。在碱性条件下(pH 10-11),在离子液体和纳米粒子的存在下开始凝胶生长过程。然后,将溶胶注入到聚丙烯空心纤维段中进行原位凝胶化过程。

在水性基质中,农药的检测限在 0.004 至 0.095 ng/mL 之间,在头发基质中为 0.003 至 0.080 ng/mL。在实际样品中,农药在卖家头发和研究人员头发中的回收率在 82.0%至 94.0%之间。结果表明,HF-SPME-HPLC-PDA 非常适用于分析生物和环境样品中的农药。

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