Cabrera Liziara da C, Caldas Sergiane S, Prestes Osmar D, Primel Ednei G, Zanella Renato
Departamento de Química, Universidade Federal de Santa Maria, Santa Maria-RS, Brazil.
Universidade Federal da Fronteira Sul - Campus Realeza, Realeza-PR, Brazil.
J Sep Sci. 2016 May;39(10):1945-54. doi: 10.1002/jssc.201501204. Epub 2016 Apr 29.
Many compounds are used for pest control during the production and storage of rice, making it necessary to employ multiclass methods for pesticide residues determination. For this purpose, QuEChERS-based methods are very efficient, fast and accurate, and improvements in the clean-up step are important, especially for complex matrices, like cereals. In this work, different sorbents such as chitosan, florisil(®) , alumina, diatomaceous earth, graphitized carbon black, besides the commonly used primary secondary amine and octadecylsilane, were evaluated for dispersive solid-phase extraction clean-up in acetate-buffered QuEChERS method for the determination of residues of 20 representative pesticides and one metabolite in rice by liquid chromatography coupled to tandem mass spectrometry. The sorbent C18 presented the best results, however, chitosan showed similar results, and the best performance among the unconventional sorbents evaluated. The method limit of quantification, attending accuracy (70-120% recovery) and precision (RSD ≤20%) criteria, ranged from 5 to 20 μg/kg. Results showed that chitosan is an effective alternative to reduce analysis costs, maintaining the method reliability and accuracy.
在大米生产和储存过程中,许多化合物被用于害虫防治,因此有必要采用多类方法来测定农药残留。为此,基于QuEChERS的方法非常高效、快速且准确,改进净化步骤很重要,特别是对于像谷物这样的复杂基质。在这项工作中,除了常用的伯仲胺和十八烷基硅烷外,还对壳聚糖、弗罗里硅土(®)、氧化铝、硅藻土、石墨化炭黑等不同吸附剂进行了评估,用于乙酸盐缓冲QuEChERS方法中的分散固相萃取净化,以通过液相色谱-串联质谱法测定大米中20种代表性农药和一种代谢物的残留量。吸附剂C18表现出最佳结果,然而,壳聚糖也显示出类似的结果,并且在所评估的非常规吸附剂中表现最佳。按照准确度(回收率70 - 120%)和精密度(相对标准偏差≤20%)标准,方法定量限为5至20 μg/kg。结果表明,壳聚糖是降低分析成本的有效替代物,同时能保持方法的可靠性和准确性。