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基于镧系元素的金属有机骨架的特性及其在辣椒中农药提取的基质固相分散程序的开发和验证中的应用,采用气相色谱-质谱法。

Characterization and application of a lanthanide-based metal-organic framework in the development and validation of a matrix solid-phase dispersion procedure for pesticide extraction on peppers (Capsicum annuum L.) with gas chromatography-mass spectrometry.

机构信息

Departamento de Química Fundamental, UFPE, Recife, PE, Brazil.

Coordenadoria de Licenciatura em Química, IFS, Aracaju, SE, Brazil.

出版信息

J Sep Sci. 2018 Apr;41(7):1593-1599. doi: 10.1002/jssc.201700812. Epub 2018 Jan 26.

Abstract

The metal-organic framework [(La Sm ) (DPA) (H O) ] was synthetized and characterized by X-ray diffractometry, differential thermogravimetric analysis, and infrared spectroscopy. The material was tested for the development and validation of a matrix solid-phase dispersion procedure for extraction of atrazine, bifenthrin, bromuconazole, clofentezine, fenbuconazole, flumetralin, procymidone, and pirimicarb, from peppers, with analysis using gas chromatography with mass spectrometry in the selected ion monitoring mode. The method developed was linear over the range tested (50.0-1000.0 μg/kg for procymidone and 200.0-1000.0 μg/kg for all other pesticides), with correlation coefficients ranging from 0.9930 to 0.9992. Experiments were carried out at 250.0, 500.0, and 1000.0 μg/kg fortification levels, and resulted in recoveries in the range of 52.7-135.0%, with coefficient of variation values between 5.2 and 5.4%, respectively, for [(La Sm ) (DPA) (H O) ] sorbent. Detection and quantification limits ranged from 16.0 to 67.0 μg/kg and from 50.0 to 200.0 μg/kg, respectively, for the different pesticides studied. The results were compared with literature data. The developed and validated method was applied to real samples. The analysis detected the presence of residues of pesticides procymidone, fenbuconazole, flumetralin, clofentezine, atrazine, and bifenthrin.

摘要

[(La Sm ) (DPA) (H O) ] 金属有机骨架通过 X 射线衍射、差示热重分析和红外光谱进行合成和表征。该材料用于开发和验证基质固相分散程序,从辣椒中提取莠去津、氟丙菊酯、溴菌唑、氯氟醚菊酯、苯醚甲环唑、氟虫脲、菌核净和吡虫啉,使用气相色谱-质谱在选择离子监测模式下进行分析。该方法在测试范围内(菌核净为 50.0-1000.0μg/kg,其他所有农药为 200.0-1000.0μg/kg)呈线性,相关系数范围为 0.9930 至 0.9992。在 250.0、500.0 和 1000.0μg/kg 加标水平进行实验,回收率在 52.7-135.0%范围内,(La Sm )(DPA)(H O ) 吸附剂的变异系数值分别在 5.2 和 5.4%之间。检测限和定量限范围分别为 16.0-67.0μg/kg 和 50.0-200.0μg/kg,用于不同研究的农药。将结果与文献数据进行比较。开发和验证的方法应用于实际样品。分析检测到残留农药菌核净、苯醚甲环唑、氟虫脲、氯氟醚菊酯、莠去津和氟丙菊酯。

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