利用低温分区萃取和气相色谱-质谱分析法测定燕麦粉中的农药残留量

IF 2.701
Aline Maria Teixeira, Maria Eliana L. R. De Queiroz, Alessandra A. Z. Rodrigues, André Fernando de Oliveira, Vitor Manuel Libardi, Jéssika Faêda de Freitas
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引用次数: 0

摘要

优化并验证了一种基于固液萃取-低温分区(SLE/LTP)和气相色谱-质谱联用(GC-MS)分析的简便方法,用于测定燕麦粉中农药三唑醇、氟虫腈、λ-氰戊菊酯、苯醚甲环唑和唑菌酯的残留量。为优化该技术并确定同时萃取分析物的最佳条件,采用了因子设计。乙腈-样品萃取及其 4 小时的冷冻使农药的回收和提取物的净化成为可能。检测限为 1.72 至 12.9 μg kg-1,定量限为 5.73 至 43.0 μg kg-1。这些数值都低于国家法律允许的最大残留限量(MRL)。回收率介于 91.7%和 108%之间,变异系数低于 12%。对从维索萨(巴西米纳斯吉拉斯州)当地市场随机获得的燕麦粉样品进行了验证,未检测到任何残留。事实证明,SLE/LTP-GC-MS 方法简单、高效、选择性强、灵敏度高,可用于测定燕麦粉样品中的农药残留,与文献中描述的技术相比,该方法更为简便。
本文章由计算机程序翻译,如有差异,请以英文原文为准。

Determination of pesticide residues in oat flour using low-temperature partition extraction and GC–MS analysis

Determination of pesticide residues in oat flour using low-temperature partition extraction and GC–MS analysis

A simple method based on solid–liquid extraction with a low-temperature partition (SLE/LTP) and analysis by gas chromatography coupled to mass spectrometry (GC–MS) was optimized and validated for determining residues of the pesticides triadimenol, flutriafol, λ-cyhalothrin, difenoconazole, and azoxystrobin in oat flour. A factorial design was employed to optimize the technique and establish the best conditions for the simultaneous extraction of the analytes. Acetonitrile-sample extraction and its 4 h freezing made it possible to recover the pesticides and clean the extracts in a single step. The limit of detection ranged from 1.72 to 12.9 μg kg−1, and the limit of quantification from 5.73 to 43.0 μg kg−1. These values are below the maximum residue limit (MRL) permitted by National legislation. The recovery percentage fell between 91.7 and 108%, with coefficients of variation under 12%. The validated method was applied to oat flour samples randomly acquired from the local market of Viçosa (Minas Gerais, Brazil) and no residues were detected. The SLE/LTP–GC–MS method proved simple, efficient, selective, and sensitive for determining pesticide residues from oat flour samples, offering a more simplified approach compared to techniques described in the literature.

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