Martins Manoel L, Kemmerich Magali, Prestes Osmar D, Maldaner Liane, Jardim Isabel C S F, Zanella Renato
Laboratory of Pesticide Residue Analysis (LARP), Chemistry Department, Federal University of Santa Maria, 97105-900 Santa Maria, RS, Brazil.
Exact Sciences Center, Chemistry Department, State University of Maringá, 87020-900 Maringá, PR, Brazil.
J Chromatogr A. 2017 Sep 8;1514:36-43. doi: 10.1016/j.chroma.2017.07.080. Epub 2017 Jul 26.
In this study, the efficiency of a new fluorinated sorbent for dispersive solid-phase extraction (d-SPE) clean-up in extracts provided by the QuEChERS (Quick, Easy, Cheap, Effective, Rugged and Safe) acetate method from tomato and sweet pepper samples was evaluated by ultra-high performance liquid chromatography tandem mass spectrometry (UHPLC-MS/MS). Clean-up using d-SPE technique has been widely used associated with the QuEChERS method. The most commonly sorbents used in d-SPE are primary secondary amine (PSA), octadecylsilane (C18) and graphitized carbon black (GCB), which are indicated to remove sugars, fatty acids, pigments, among others. The performance of an alternative fluorinated sorbent was compared with PSA and C18 sorbents for representative pesticides and better results were obtained when the fluorinated sorbent was used. Validation presented acceptable results for trueness and precision, with method limit of detection between 0.9 and 1.8μgkg and limit of quantification from 2.6 to 5.4μgkg. Most of the compounds presented low matrix effect. Results showed that the fluorinated sorbent contribute to the clean-up of the tomato extract and is an effective alternative, with lower costs and greater efficiency. Commercial tomato samples were analyzed using the proposed method and residues of dimethoate, tetraconazole and thiamethoxam were detected.
在本研究中,采用超高效液相色谱串联质谱法(UHPLC-MS/MS)评估了一种新型氟化吸附剂用于分散固相萃取(d-SPE)净化番茄和甜椒样品中由QuEChERS(快速、简便、廉价、高效、耐用和安全)乙酸盐法提供的提取物的效率。使用d-SPE技术进行净化已与QuEChERS方法广泛联用。d-SPE中最常用的吸附剂是伯仲胺(PSA)、十八烷基硅烷(C18)和石墨化炭黑(GCB),它们可用于去除糖、脂肪酸、色素等。将一种替代的氟化吸附剂与PSA和C18吸附剂用于代表性农药的性能进行了比较,结果表明使用氟化吸附剂时获得了更好的效果。验证显示准确性和精密度结果可接受,方法的检测限在0.9至1.8μg/kg之间,定量限在2.6至5.4μg/kg之间。大多数化合物呈现出较低的基质效应。结果表明,氟化吸附剂有助于净化番茄提取物,是一种有效的替代方法,成本更低且效率更高。使用所提出的方法对市售番茄样品进行了分析,检测到了乐果、四氟醚唑和噻虫嗪的残留。