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一种通过超高效液相色谱-串联质谱法测定土壤中咪唑啉酮类除草剂的简单高效方法。

A simple and efficient method for imidazolinone herbicides determination in soil by ultra-high performance liquid chromatography-tandem mass spectrometry.

作者信息

Kemmerich Magali, Bernardi Gabrieli, Adaime Martha B, Zanella Renato, Prestes Osmar D

机构信息

Laboratory of Pesticide Residue Analysis (LARP), Chemistry Department, Federal University of Santa Maria, 97105-900 Santa Maria, RS Brazil.

Laboratory of Pesticide Residue Analysis (LARP), Chemistry Department, Federal University of Santa Maria, 97105-900 Santa Maria, RS Brazil.

出版信息

J Chromatogr A. 2015 Sep 18;1412:82-9. doi: 10.1016/j.chroma.2015.08.005. Epub 2015 Aug 6.

Abstract

The use of pesticides in agriculture has generated numerous consequences to the environment, requiring analysis of the persistent residues in soil, water and air. The variability of soil properties interferes in the extraction of pesticide residues with robustness and accuracy. The group of imidazolinones herbicides, widely used for weed control, becomes an additional task in multiresidue extraction procedures because of their low pKa values. In order to determine these compounds in soil samples, different methods have been proposed, however they can be very laborious and require more time and well trained analysts. Thus, this study aimed to develop a simple and efficient method for determination of imidazolinones (imazamox, imazapic, imazapyr, imazaquin and imazethapyr) residues in soil, using an extraction with aqueous ammonium acetate solution (0.5 M) and clean-up with dispersive solid phase extraction employing PSA, followed by UHPLC-MS/MS analysis. Satisfactory values of accuracy (70-93%) and RSD (≤17%) were achieved, as well as lower limit of quantification (5.0 μg kg(-1)). Considering the matrix and compounds complexity, the developed and validated method proved to be an excellent tool for rapid analysis (20 min), with reliability for application in real samples with wide pH range. In the analysis of 22 real samples, the method allowed the quantification of imazapic (5.84 and 12.1 μg kg(-1)), imazapyr (5.3 μg kg(-1)) and imazethapyr (24.0 and 37.7 μg kg(-1)) in three samples.

摘要

农业中使用农药已对环境产生了诸多影响,这就需要对土壤、水和空气中的持久性残留物进行分析。土壤性质的变异性会影响农药残留的提取,使其难以稳健且准确地进行。咪唑啉酮类除草剂因广泛用于杂草控制,且其pKa值较低,在多残留提取程序中成为一项额外任务。为了测定土壤样品中的这些化合物,人们提出了不同的方法,但这些方法可能非常繁琐,需要更多时间且分析人员要训练有素。因此,本研究旨在开发一种简单高效的方法来测定土壤中咪唑啉酮类(甲氧咪草烟、咪草酸、吡唑嘧磺隆、咪唑喹啉酸和咪唑乙烟酸)残留物,方法是先用0.5 M醋酸铵水溶液进行提取,然后采用PSA进行分散固相萃取净化,接着进行超高效液相色谱-串联质谱分析。该方法获得了令人满意的准确度值(70 - 93%)和相对标准偏差(≤17%),以及较低的定量限(5.0 μg kg⁻¹)。考虑到基质和化合物的复杂性,所开发和验证的方法被证明是一种快速分析(20分钟)的出色工具,适用于pH范围广泛的实际样品。在对22个实际样品的分析中,该方法在三个样品中定量出了咪草酸(5.84和12.1 μg kg⁻¹)、吡唑嘧磺隆(5.3 μg kg⁻¹)和咪唑乙烟酸(24.0和37.7 μg kg⁻¹)。

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