磁分散微固相萃取与中空纤维液相微萃取相结合预富集水样中的痕量毒死蜱农药

IF 2.2 4区 化学 Q3 CHEMISTRY, MULTIDISCIPLINARY Journal of the Iranian Chemical Society Pub Date : 2024-05-14 DOI:10.1007/s13738-024-03028-4
Reyhaneh Kouchakinejad, Shahab Shariati, Jafar Abolhasani, Ebrahim Ghorbani Kalhor, Mohammad Taghi Vardini, Ameneh Dorri
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引用次数: 0

摘要

本研究将磁性分散微固相萃取(MD-µSPE)与中空纤维液相微萃取(HF-LPME)相结合,在气相色谱-质谱联用(GC/MS)前对毒死蜱农药进行预浓缩和痕量测定。用磁铁矿纳米颗粒负载蕨类植物 Azolla filiculoides 生物质,制备磁性吸附剂(azolla@Fe3O4)。利用 FESEM、TEM、VSM、FTIR、EDX 和 XRD 方法研究了所制备的磁性纳米复合材料(MNCs)的结构特征。在拟议的 MD-µSPE/HF-LPME 方法中,MD-µSPE 步骤中的吸附/解吸变量通过田口分数因子设计进行了优化。毒死蜱在MD-µSPE的优化条件(样品体积=50 mL,接触时间=15 min,溶液pH=3,吸附剂质量=0.05 g,离子强度=0.01 mol L-1,洗脱剂类型=乙醇)下吸附后,将2.0 mL解吸后的乙醇溶液加入16 mL 10%(w/v)NaCl水溶液中进行下一步HF-LPME方法的测定,最后采用GC/MS进行分析。该方法的检出限为 0.05 μg L-1,定量限为 0.5 μg L-1,动态线性范围为 0.5-1000.0 μg L-1,预浓缩因子在 700-1050 之间,重复性(RSD%)为 6.9%。通过测定实际样品中的毒死蜱,证实了 MD-µSPE/HF-LPME 方法的适用性,相对回收率在 97.0-108.5% 之间。结果表明所开发的 MD-µSPE/HF-LPME 方法具有良好的准确度和精密度,可用于水样中痕量毒死蜱的预浓缩和测定。
本文章由计算机程序翻译,如有差异,请以英文原文为准。

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Magnetic dispersive micro-solid-phase extraction integrated with hollow fiber liquid-phase microextraction for preconcentration of trace amounts of chlorpyrifos pesticide in aqueous samples

In the present study, the integration of magnetic dispersive micro-solid-phase extraction (MD-µSPE) with hollow fiber liquid-phase microextraction (HF-LPME) prior to gas chromatography–mass spectrometry (GC/MS) was developed to preconcentrate and determine trace amounts of chlorpyrifos pesticide. Azolla filiculoides fern biomass was loaded by magnetite nanoparticles to prepare magnetic adsorbent (azolla@Fe3O4). The structural characteristics of the produced magnetic nanocomposites (MNCs) were investigated by FESEM, TEM, VSM, FTIR, EDX, and XRD methods. In the proposed MD-µSPE/HF-LPME method, the adsorption/desorption variables in MD-µSPE step were optimized by Taguchi fractional factorial design. After chlorpyrifos adsorption in the optimized condition of MD-µSPE (Vsample = 50 mL, contact time = 15 min, solution pH = 3, adsorbent mass = 0.05 g, ionic strength = 0.01 mol L−1, and eluent type = ethanol), 2.0 mL of the desorbed ethanolic solution was added to 16 mL of 10% (w/v) NaCl aqueous solution for the next HF-LPME method and the final analysis was performed by GC/MS. The developed method showed a limit of detection of 0.05 μg L−1, a limit of quantification of 0.5 μg L−1, a dynamic linear range of 0.5–1000.0 μg L−1, preconcentration factors between 700 and 1050, and a repeatability (RSD%) of 6.9%. The suitability of the MD-µSPE/HF-LPME method was confirmed by measuring chlorpyrifos in real samples with relative recoveries in the range of 97.0–108.5%. The results showed good accuracy and precision of the developed MD-µSPE/HF-LPME method for the preconcentration and determination of trace amounts of chlorpyrifos in the aqueous samples.

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来源期刊
CiteScore
4.40
自引率
8.30%
发文量
230
审稿时长
5.6 months
期刊介绍: JICS is an international journal covering general fields of chemistry. JICS welcomes high quality original papers in English dealing with experimental, theoretical and applied research related to all branches of chemistry. These include the fields of analytical, inorganic, organic and physical chemistry as well as the chemical biology area. Review articles discussing specific areas of chemistry of current chemical or biological importance are also published. JICS ensures visibility of your research results to a worldwide audience in science. You are kindly invited to submit your manuscript to the Editor-in-Chief or Regional Editor. All contributions in the form of original papers or short communications will be peer reviewed and published free of charge after acceptance.
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