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分散固相萃取法用于从土壤、植物和水样中预浓缩对硫磷乙基作为沙林神经毒剂的模拟物,然后进行 GC-MS 测定。

Development of dispersive solid phase extraction method for the preconcentration of parathion ethyl as a simulant of nerve agent sarin from soil, plant and water samples prior to GC-MS determination.

机构信息

Chemistry Department, Yıldız Technical University, 34220, Istanbul, Türkiye.

Faculty of Pharmacy, Department of Analytical Chemistry, İstinye University, 34010, Istanbul, Türkiye.

出版信息

Environ Monit Assess. 2024 Aug 21;196(9):829. doi: 10.1007/s10661-024-13007-0.

DOI:10.1007/s10661-024-13007-0
PMID:39167268
Abstract

In the presented study, an efficient and fast analytical method was developed for the determination of parathion ethyl as sarin simulant by gas chromatography-mass spectrometry (GC-MS). Dispersive solid phase extraction (DSPE) was performed to concentrate parathion ethyl from soil, plant and water samples. Reduced graphene oxide-iron (II, III) oxide (rGO-FeO) nanocomposite was used as an adsorbent to collect the target analyte from the aqueous sample solutions. After the optimization of extraction/preconcentration parameters, optimum conditions for adsorbent amount, eluent type, mixing type/period, eluent volume and initial sample volume were determined as 15 mg, acetonitrile, vortex/30 s, 100 µL and 10 mL, respectively. Under the optimum conditions, analytical performance of the developed DSPE-GC-MS method was evaluated in terms of limit of detection (LOD), limit of quantitation (LOQ) and dynamic range. Dynamic range, LOD and LOQ values were figured out to be 0.94-235.15 µg/kg, 0.41 µg/kg and 1.36 µg/kg (mass based), respectively. Satisfactory percent recovery results (90.3-125% for soil, 93.5-108.7% for plant, 88.5-112.9% for tap water) were achieved for soil, plant and tap water samples which proved the accuracy and applicability of the developed method. It is predicted that the DSPE-GC-MS method can be accurately used for the detection of sarin in soil, plant and water samples taken from war territories.

摘要

在本研究中,开发了一种通过气相色谱-质谱联用仪(GC-MS)测定作为沙林模拟物的乙基对硫磷的高效快速分析方法。分散固相萃取(DSPE)用于从土壤、植物和水样中浓缩乙基对硫磷。还原氧化石墨烯-铁(II、III)氧化物(rGO-FeO)纳米复合材料被用作吸附剂,从水样中收集目标分析物。在优化了提取/预浓缩参数后,确定了吸附剂用量、洗脱剂类型、混合类型/周期、洗脱剂体积和初始样品体积的最佳条件分别为 15mg、乙腈、涡旋/30s、100µL 和 10mL。在最佳条件下,从检出限(LOD)、定量限(LOQ)和动态范围三个方面评估了所开发的 DSPE-GC-MS 方法的分析性能。得出的动态范围、LOD 和 LOQ 值分别为 0.94-235.15µg/kg、0.41µg/kg 和 1.36µg/kg(基于质量)。对于土壤、植物和自来水样品,均获得了令人满意的回收率结果(土壤为 90.3-125%,植物为 93.5-108.7%,自来水为 88.5-112.9%),证明了所开发方法的准确性和适用性。预计该 DSPE-GC-MS 方法可准确用于检测来自战区的土壤、植物和水样中的沙林。

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