This work proposes a novel Quick, Easy, Cheap, Effective, Rugged, and Safe (QuEChERS) method in combination with ultra-high performance liquid chromatography-tandem mass spectrometry for the determination of sulfonylurea residues in edible seeds. The chromatographic separation of nine sulfonylureas was accomplished in less than 5.5 min, using a Luna Omega C18 column (50 × 2.1 mm, 1.6 µm). Mobile phase was supplied at 0.55 mL min-1 and consisted of 0.01% (v/v) aqueous acetic acid as eluent A and a mixture methanol/acetonitrile (80/20, v/v) as eluent B. Column temperature was established at 25 °C. A QuEChERS procedure was investigated as sample treatment for sulfonylureas extraction and sample clean-up. Different clean-up agents (i.e. PSA, Z-Sep+, EMR-Lipid and C18) were evaluated, selecting Z-Sep+ (25 mg) as the best option. The proposed method provided an extraction efficiency greater than 86.2%, while absolute matrix effect was lower than 50.1%. Matrix-matched calibration curves were required for analyte quantification. The analytical method was characterized according to SANTE/11813/2017 guideline, and including limits of detection and quantification, precision, and trueness. Linear dynamic ranges were established from 5 to 150 µg kg-1 for all analytes. Linearity (R2 ≥ 0.9974) and precision in terms of repeatability and intermediate precision (relative standard deviation ≤ 14.7%) are reported. The reporting limit was established at 5 µg kg-1, which is above the limits of quantification of the proposed method (≤ 1.64 µg kg-1) and below the maximum residue levels currently established by European legislation. In general, trueness is within the range of 70-120%. Despite greater recoveries were obtained at the reporting limit (i.e. 120-138%), relative standard deviations lower than 20% were obtained at this concentration level, so fulfilling the requirements of SANTE/11813/2017 guideline. This work represents the first analytical method intended for the analysis of sulfonylureas in sunflower, pumpkin and chia seeds, which are complex matrices due to their high content of fat as well as of growing interest due to their current commercialization as nutraceuticals.

中文翻译：

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QuEChERS结合超高效液相色谱-串联质谱法测定用作营养食品的食用种子中的磺酰脲类农药残留。

这项工作提出了一种新颖，快速，简便，便宜，有效，坚固和安全的方法（QuEChERS），结合超高效液相色谱-串联质谱法测定可食用种子中的磺酰脲残留量。使用Luna Omega C18色谱柱（50×2.1 mm，1.6 µm），在不到5.5分钟的时间内完成了九种磺酰脲的色谱分离。流动相的进样量为0.55 mL min-1，由0.01％（v / v）的乙酸水溶液作为洗脱剂A和甲醇/乙腈的混合物（80/20，v / v）作为洗脱剂B。柱温设定为25℃。研究了QuEChERS程序作为磺酰脲类提取物和样品净化的样品处理方法。评估了不同的清洁剂（即PSA，Z-Sep +，EMR-Lipid和C18），选择Z-Sep +（25 mg）作为最佳选择。所提方法的萃取效率大于86.2％，而绝对基质效应小于50.1％。基质匹配的校准曲线是分析物定量所必需的。该分析方法根据SANTE / 11813/2017指南进行了表征，包括检测和定量的极限，精度和真实性。所有分析物的线性动态范围设定为5至150 µg kg-1。报告了线性（R2≥0.9974）和在重复性和中间精度方面的精度（相对标准偏差≤14.7％）。报告限度设定为5 µg kg-1，高于建议的方法的定量限（≤1.64 µg kg-1），并且低于欧洲法规目前确定的最大残留量。通常，真实度在70-120％的范围内。尽管在报告限值（即120％至138％）处获得了更高的回收率，但在此浓度水平下仍获得了低于20％的相对标准偏差，因此符合SANTE / 11813/2017准则的要求。这项工作代表了用于分析向日葵，南瓜和奇亚籽中磺酰脲的第一种分析方法，这些磺酰脲类是复杂的基质，因为它们的脂肪含量很高，并且由于它们目前作为营养保健品的商业化而日益受到关注。