European Commission, Joint Research Centre, Institute for Reference Materials and Measurements (IRMM), Retieseweg 111, 2440 Geel, Belgium.
European Commission, Joint Research Centre, Institute for Reference Materials and Measurements (IRMM), Retieseweg 111, 2440 Geel, Belgium.
Food Chem. 2012 May 1;132(1):567-73. doi: 10.1016/j.foodchem.2011.10.071. Epub 2011 Oct 30.
The feasibility for producing a matrix reference material for selected pesticides in a carrot/potato matrix was investigated. A commercially available baby food (carrot/potato-based mash) was spiked with 11 pesticides at the respective EU maximum residue limits (MRLs), and further processed by either freezing or freeze-drying. Batches of some 150 units were produced per material type. First, the materials were assessed for the relative amount of pesticide recovered after processing (ratio of pesticide concentration in the processed material to the initially spiked pesticide concentration). In addition, the materials' homogeneity (bottle-to-bottle variation), and the short-term (1 month) and mid-term (5 months) stability at different temperatures were assessed. For this, an in-house validated GC-EI-MS method operated in the SIM mode with a sample preparation procedure based on the QuEChERS ("quick, easy, cheap, effective, rugged, and safe") principle was applied. Measurements on the frozen material provided the most promising results (smallest analyte losses during production), and also freeze-drying proved to be a suitable alternative processing technique for most of the investigated pesticides. Both the frozen and the freeze-dried material showed to be sufficiently homogeneous for the intended use, and storage at -20°C for 5 months did not reveal any detectable material degradation. The results constitute an important step towards the development of a pesticide matrix reference material.
研究了在胡萝卜/马铃薯基质中制备选定农药基质参考物质的可行性。将市售的婴儿食品(基于胡萝卜/马铃薯的糊状物)用 11 种农药以欧盟最大残留限量(MRL)进行加标,然后通过冷冻或冻干进一步加工。每种材料类型生产约 150 个单位。首先,评估了加工后农药回收的相对量(加工材料中农药浓度与初始加标农药浓度的比值)。此外,还评估了材料的均一性(瓶间变化)以及在不同温度下的短期(1 个月)和中期(5 个月)稳定性。为此,应用了基于 QuEChERS(“快速、简便、廉价、有效、耐用和安全”)原理的 GC-EI-MS 方法,该方法在 SIM 模式下操作,并进行了样品制备程序的内部验证。冷冻材料的测量结果最有希望(生产过程中分析物损失最小),而且冻干也被证明是大多数研究农药的合适替代加工技术。冷冻和冻干材料均表现出足够的均一性,适合预期用途,在-20°C 下储存 5 个月未发现任何可检测到的材料降解。这些结果是开发农药基质参考物质的重要一步。