College of Science, China Agricultural University, Beijing 100193, China.
Pesticide Safety Evaluation Research Center, Institute for Agro-food Standards and Testing Technology, Shanghai Academy of Agricultural Sciences, Shanghai 201106, China.
Food Chem. 2019 Mar 15;276:140-146. doi: 10.1016/j.foodchem.2018.10.019. Epub 2018 Oct 4.
Cinnamon bark is a very complex spices matrix for pesticide residue analysis. In this study, two cleanup procedures, dispersive solid-phase extraction (d-SPE) and repetitive d-SPE, combined with Quick, Easy, Cheap, Effective, Rugged and Safe (QuEChERS) extraction were both investigated and applied for the determination of 60 pesticide residues in cinnamon bark by liquid chromatography - tandem mass spectrometry (LC-MS/MS) detection. The extraction solvents, phase partition salts, and cleanup sorbents were optimized. The results showed that 150 mg MgSO + 50 mg C showed the best performance in d-SPE. The repetitive d-SPE achieved less matrix effects than d-SPE, but several high water-solubility analytes were lost during the cleanup, and also the 10 fold dilution compromised the sensitivities of analytes. With the validated QuEChERS-d-SPE method, 44 of 60 pesticides obtained satisfactory recoveries (71%-118%) and RSDs (2%-27%) at three to five spiking levels. The method was applied to monitor 15 market cinnamon samples.
肉桂皮是一种非常复杂的香料基质，用于农药残留分析。在这项研究中，两种净化程序，分散固相萃取（d-SPE）和重复 d-SPE，与快速、简单、廉价、有效、坚固和安全（QuEChERS）提取相结合，都被研究并应用于通过液相色谱-串联质谱（LC-MS/MS）检测测定肉桂皮中的 60 种农药残留。优化了提取溶剂、相分配盐和净化吸附剂。结果表明，在 d-SPE 中，150mg MgSO+50mg C 表现出最佳性能。重复 d-SPE 比 d-SPE 产生的基质效应更小，但在净化过程中会损失一些高水溶性分析物，并且 10 倍稀释也会影响分析物的灵敏度。采用经过验证的 QuEChERS-d-SPE 方法，在三个至五个加标水平下，60 种农药中的 44 种获得了令人满意的回收率（71%-118%）和 RSD（2%-27%）。该方法应用于监测 15 个市场肉桂样品。
