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气相色谱-质谱联用法测定番木瓜和鳄梨样品中农药的基质效应和不确定度的验证与评估。

Validation and assessment of matrix effect and uncertainty of a gas chromatography coupled to mass spectrometry method for pesticides in papaya and avocado samples.

机构信息

Facultad de Ciencias Químicas, Universidad de Colima, Colima, Mexico.

Facultad de Ciencias, Universidad de Colima, Colima, Mexico.

出版信息

J Food Drug Anal. 2017 Jul;25(3):501-509. doi: 10.1016/j.jfda.2016.09.005. Epub 2016 Nov 5.

Abstract

In this paper a method of using the "quick, easy, cheap, effective, rugged, and safe" (QuEChERS) extraction and gas chromatography coupled to mass spectrometry detection (GC-MS) was developed for the analysis of five frequently applied pesticides in papaya and avocado. The selected pesticides, ametryn, atrazine, carbaryl, carbofuran, and methyl parathion, represent the most commonly used classes (carbamates, organophosphorous, and triazines). Optimum separation achieved the analysis of all pesticides in < 6.5 minutes. Validation using papaya and avocado samples established the proposed method as linear, accurate, and precise. In this sense, the correlation coefficients were > 0.99. The limits of detection (LOD) and quantification (LOQ) in papaya ranged from 0.03 mg/kg to 0.35 mg/kg and from 0.06 mg/kg to 0.75 mg/kg, respectively. Meanwhile for avocado, LOD values varied from 0.14 mg/kg to 0.28 mg/kg and LOQ values ranged from 0.22 mg/kg to 0.40 mg/kg. Recoveries obtained for each pesticide in both matrices ranged between 60.6% and 104.3%. The expanded uncertainty of the method was < 26% for all the pesticides in both fruits. Finally, the method was applied to other fruits.

摘要

本文开发了一种使用“快速、简便、廉价、有效、耐用和安全”(QuEChERS)提取和气相色谱-质谱联用(GC-MS)检测法分析木瓜和鳄梨中五种常用农药的方法。选择的农药莠去津、莠去津、西玛津、克百威和甲基对硫磷代表了最常用的类别(氨基甲酸酯类、有机磷类和三嗪类)。最佳分离条件可在 < 6.5 分钟内完成所有农药的分析。使用木瓜和鳄梨样品进行验证,证明了所提出的方法具有线性、准确性和精密度。在这种情况下,相关系数> 0.99。在木瓜中的检测限(LOD)和定量限(LOQ)范围分别为 0.03-0.35 mg/kg 和 0.06-0.75 mg/kg;而在鳄梨中,LOD 值范围为 0.14-0.28 mg/kg,LOQ 值范围为 0.22-0.40 mg/kg。在两种基质中,每种农药的回收率均在 60.6%-104.3%之间。该方法在两种水果中所有农药的扩展不确定度均< 26%。最后,该方法被应用于其他水果。

https://cdn.ncbi.nlm.nih.gov/pmc/blobs/dae1/9328818/3b027656af64/jfda-25-03-501f1.jpg

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本文引用的文献

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Electrochemical determination of paraquat in citric fruit based on electrodeposition of silver particles onto carbon paste electrode.
J Food Drug Anal. 2015 Sep;23(3):463-471. doi: 10.1016/j.jfda.2015.03.003. Epub 2015 May 19.
2
QuEChERS sample preparation for the determination of pesticides and other organic residues in environmental matrices: a critical review.
Anal Bioanal Chem. 2014 Jul;406(17):4089-116. doi: 10.1007/s00216-014-7798-4. Epub 2014 Apr 27.
8

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