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采用纤维状固相萃取与气相色谱-质谱联用技术测定部分蔬菜中的有机磷农药残留

Application of fabric phase sorptive extraction with gas chromatography and mass spectrometry for the determination of organophosphorus pesticides in selected vegetable samples.

机构信息

Department of Chemistry, Punjabi University, Patiala, India.

International Forensic Research Institute, Department of Chemistry and Biochemistry, Florida International University, Miami, FL, USA.

出版信息

J Sep Sci. 2019 Feb;42(4):862-870. doi: 10.1002/jssc.201800854. Epub 2019 Jan 15.

Abstract

In the present work, a high-efficiency and solvent minimized microextraction technique, fabric phase sorptive extraction followed by gas chromatography and mass spectrometry analysis is proposed for the rapid determination of four organophosphorus pesticides (terbufos, malathion, chlorpyrifos, and triazofos) in vegetable samples including beans, tomato, brinjal, and cabbage. Fabric phase sorptive extraction combines the beneficial features of sol-gel derived microextraction sorbents with the rich surface chemistry of cellulose fabric substrate, which collectively form a highly efficient microextraction system. Fabric phase sorptive extraction membrane, when immersed directly into the sample matrix, may extract target analytes even when high percentage of matrix interferents are present. The technique also greatly simplifies sample preparation workflow. Most important fabric phase sorptive extraction parameters were investigated and optimized. The developed method displayed good linearity over the concentration range 0.5-500 ng/g. Under optimum experimental conditions, the limits of detection were found in the range of 0.033 to 0.136 ng/g. The relative standard deviations for the extraction of organophosphorus pesticides were < 5%. Subsequently, the new method was applied to beans, tomato, brinjal, and cabbage samples. The results from the real sample analysis indicate that the method is green, rapid, and economically feasible for the determination of organophosphorus pesticides in vegetable samples.

摘要

在本工作中,提出了一种高效、溶剂用量最小的微萃取技术,即纤维状固相萃取,随后进行气相色谱和质谱分析,用于快速测定蔬菜样品(包括豆类、番茄、茄子和白菜)中的四种有机磷农药(特丁磷、马拉硫磷、毒死蜱和三唑磷)。纤维状固相萃取将溶胶-凝胶衍生的微萃取吸附剂的优点与纤维素织物基底丰富的表面化学结合在一起,共同构成了一种高效的微萃取系统。纤维状固相萃取膜直接浸入样品基质中时,即使存在大量基质干扰物,也可以提取目标分析物。该技术还大大简化了样品制备工作流程。对纤维状固相萃取的最重要参数进行了考察和优化。所开发的方法在 0.5-500 ng/g 的浓度范围内显示出良好的线性。在最佳实验条件下,发现有机磷农药的检出限在 0.033 到 0.136 ng/g 范围内。有机磷农药萃取的相对标准偏差均小于 5%。随后,将新方法应用于豆类、番茄、茄子和白菜样品。实际样品分析结果表明,该方法绿色、快速且经济可行,可用于蔬菜样品中有机磷农药的测定。

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