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基于填充注射器中天然纳米硅藻土的固相萃取结合气相色谱-质谱法测定水样中的三种有机氯农药

Determination of Three Organochlorine Pesticides in Aqueous Samples by Solid-Phase Extraction Based on Natural Nano Diatomite in Packed Syringe Coupled to Gas Chromatography-Mass Spectrometry.

作者信息

Taghani Abdollah, Goudarzi Nasser, Bagherian Ghadamali, Chamjangali Mansour Arab

机构信息

Faculty of Chemistry, Shahrood University of Technology.

出版信息

Anal Sci. 2017;33(10):1135-1140. doi: 10.2116/analsci.33.1135.

Abstract

A rapid, simple, and sensitive technique is proposed based on a miniaturized solid-phase extraction method named mictroextraction in a packed syringe coupled with gas chromatography-mass spectrometry for the preconcentration and determination of three organochlorine pesticides. These include hexachlorobenzene, heptachlor and aldrine in aqueous samples. For the first time, the natural nano diatomite is used a sorbent. Based on this technique, 6.0 mg of the nano sorbent is inserted in a syringe between two polypropylene frits. The analytes would be adsorbed on the solid phase, and would subsequently be eluted using organic solvents. The influence of some important parameters, such as the solution pH, type and volume of the organic desorption solvent, and amount of sorbent on the extraction efficiency of the selected pesticides, is investigated. The proposed method shows good linearity in the range of 0.1 - 40.0 μg L, and at low limits of detection in the range of 0.02 - 0.13 μg L using the selected ion-monitoring mode. The reproducibility of this method was found to be in the range of 3.5 - 11.1% for the understudied pesticides. In order to evaluate the matrix effect, the developed method is also applied to the preconcentration and determination of the selected pesticides in different water samples.

摘要

基于一种名为填充注射器微萃取的小型化固相萃取方法,结合气相色谱 - 质谱联用技术,提出了一种快速、简单且灵敏的技术,用于对三种有机氯农药进行预浓缩和测定。这些农药包括水样中的六氯苯、七氯和艾氏剂。首次使用天然纳米硅藻土作为吸附剂。基于该技术,将6.0毫克纳米吸附剂插入两个聚丙烯筛板之间的注射器中。分析物将吸附在固相上,随后用有机溶剂洗脱。研究了一些重要参数,如溶液pH值、有机解吸溶剂的类型和体积以及吸附剂用量对所选农药萃取效率的影响。所提出的方法在0.1 - 40.0 μg/L范围内具有良好的线性,在选择离子监测模式下,检测限低至0.02 - 0.13 μg/L。对于所研究的农药,该方法的重现性在3.5 - 11.1%范围内。为了评估基质效应,所开发的方法还应用于不同水样中所选农药的预浓缩和测定。

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