Santilio Angela, Girolimetti Silvana, Picardo Valentina
Department of Environment and Health, National Institute of Health, Rome, Italy.
J Environ Sci Health B. 2022;57(3):184-191. doi: 10.1080/03601234.2022.2042153. Epub 2022 Mar 3.
Rapid, sensitive and selective method was studied for the determination of glyphosate in rice and wheat flour using a Raptor Polar column. Samples were extracted with acidified methanol solution. Isotope labeled internal standard was added with the extraction solvent to ensure accurate tracking and quantitation. The glyphosate was analyzed by liquid chromatography tandem mass spectrometry using a Raptor Polar column. Method performance was evaluated through a series of parameters that include accuracy, precision, linearity, limit of detection (LOD), limit of quantitation (LOQ) and matrix effect. Mean recoveries for all matrices were within 96-116% at three fortification levels. Precision for replicates was ≤19% relative standard deviation (RSD%) for wheat and ≤9% RSD% for rice across all fortification levels. Linearity was good for both matrices with a correlation coefficient >0.999 and residual <20% in the concentration range 0.025-1 mg kg. LOD was 0.005 mg kgfor both rice and wheat flour and the LOQ was 0.05 mg kgfor both matrices. The matrix effect was also studied. A successful method for the analysis of glyphosate in wheat and rice flour assure that the criteria of acceptability of the maximum residue levels (MRLs) are insured.
研究了一种使用Raptor Polar柱测定大米和小麦粉中草甘膦的快速、灵敏且选择性好的方法。样品用酸化甲醇溶液萃取。在萃取溶剂中加入同位素标记内标以确保准确追踪和定量。使用Raptor Polar柱通过液相色谱串联质谱法分析草甘膦。通过包括准确度、精密度、线性、检测限（LOD）、定量限（LOQ）和基质效应在内的一系列参数评估方法性能。在三个加标水平下，所有基质的平均回收率在96% - 116%之间。在所有加标水平下，小麦重复样的精密度相对标准偏差（RSD%）≤19%，大米的RSD%≤9%。两种基质的线性均良好，相关系数>0.999，在0.025 - 1 mg/kg浓度范围内残差<20%。大米和小麦粉的LOD均为0.005 mg/kg，两种基质的LOQ均为0.05 mg/kg。还研究了基质效应。一种成功分析小麦和大米粉中草甘膦的方法确保了最大残留限量（MRLs）可接受标准得以保证。
