Mohammad Nazari Koloujeh, Mortaza Iranifam, Ali Akbar Fathi, Mir Ali Farajzadeh, Mohammad Reza Afshar Mogaddam
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The mixture was aspirated into a syringe and then rapidly injected into 5-mL sodium chloride solution (4%, <i>w/v</i>). The resulting cloudy solution was centrifuged and 1 µL of the settled phase was used in the analysis step. The validity of the method was assessed after optimizing the experimental conditions. The obtained results showed that the limits of detection (LOD) and quantification (LOQ) for the analytes were in the ranges of 0.08–0.48 and 0.29–1.4 ng mL<sup>−1</sup>, respectively. The calibration graphs were linear in the range of 1.4–3000 ng mL<sup>−1</sup> with a coefficient of determination (<i>r</i><sup>2</sup>) ≥ 0.991. The relative standard deviations (RSDs) for replicate analyses were ≤ 5.2%. The enrichment factors (EFs) and extraction recoveries (ERs) for the studied analytes were in the ranges of 365–405 and 73–81%, respectively. 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引用次数: 0
摘要
采用分散固相萃取法提取草莓样品中的农药。该方法与分散液液微萃取相结合,进一步富集样品。为此,将5mg合成的纳米复合材料用于从5ml样品溶液中提取分析物,在搅拌下涡流8分钟。离心(5000rpm,离心3分钟)后,除去上清。然后,将吸附的分析物用1.0 mL乙醇超声洗脱。然后将混合物在5000 rpm下离心3 min,将洗脱液转移到另一个微管中,与80µL氯仿混合。将混合物吸入注射器中,快速注入5 ml氯化钠溶液(4%,w/v)。将所得混浊溶液离心,取1µL沉淀相用于分析步骤。通过对实验条件的优化,评价了该方法的有效性。结果表明,分析物的检出限(LOD)和定量限(LOQ)分别为0.08 ~ 0.48和0.29 ~ 1.4 ng mL−1。校正曲线在1.4 ~ 3000 ng mL−1范围内呈线性,决定系数(r2)≥0.991。重复分析的相对标准偏差(rsd)≤5.2%。富集因子(EFs)和萃取回收率(ERs)分别为365 ~ 405和73 ~ 81%。用该方法对几个草莓样品进行了试验,结果表明,样品中不含所研究的农药。
Development of COF@MOF Nanocomposite-Based Dispersive Solid-Phase Microextraction for the Extraction of Pesticides from Strawberries
A dispersive solid-phase extraction approach was developed for extracting certain pesticides from strawberry samples. This method was combined with dispersive liquid–liquid microextraction to further enrich the samples. To achieve this, 5 mg of the synthesized nanocomposite was used for the extraction of the analytes from 5 mL of the sample solution under agitation by vortexing for 8 min. After centrifugation (at 5000 rpm for 3 min), the supernatant was removed. Then, the adsorbed analytes were eluted with 1.0 mL of ethanol using ultrasonication. The mixture was then centrifuged at 5000 rpm for 3 min, and the eluent was transferred into another microtube and mixed with 80 µL of chloroform. The mixture was aspirated into a syringe and then rapidly injected into 5-mL sodium chloride solution (4%, w/v). The resulting cloudy solution was centrifuged and 1 µL of the settled phase was used in the analysis step. The validity of the method was assessed after optimizing the experimental conditions. The obtained results showed that the limits of detection (LOD) and quantification (LOQ) for the analytes were in the ranges of 0.08–0.48 and 0.29–1.4 ng mL−1, respectively. The calibration graphs were linear in the range of 1.4–3000 ng mL−1 with a coefficient of determination (r2) ≥ 0.991. The relative standard deviations (RSDs) for replicate analyses were ≤ 5.2%. The enrichment factors (EFs) and extraction recoveries (ERs) for the studied analytes were in the ranges of 365–405 and 73–81%, respectively. The developed method was performed on several strawberry samples and the results showed that the samples were free of the studied pesticides.
期刊介绍:
Food Analytical Methods publishes original articles, review articles, and notes on novel and/or state-of-the-art analytical methods or issues to be solved, as well as significant improvements or interesting applications to existing methods. These include analytical technology and methodology for food microbial contaminants, food chemistry and toxicology, food quality, food authenticity and food traceability. The journal covers fundamental and specific aspects of the development, optimization, and practical implementation in routine laboratories, and validation of food analytical methods for the monitoring of food safety and quality.