National Referral Laboratory, ICAR National Research Centre for Grapes, P.O. Manjri Farm, Pune 412 307, India.
Waters Corporation, Milford, MA 01757, United States.
Food Chem. 2019 Dec 15;301:125216. doi: 10.1016/j.foodchem.2019.125216. Epub 2019 Jul 23.
An improved liquid chromatography tandem mass spectrometry method is reported for the determination of residues of captan (+tetrahydrophthalimide), captafol, folpet (+phthalimide), and iprodione in fruits and vegetables. The optimized electrospray ionization parameters (high cone gas flow, and a low desolvation temperature) did not result in degradation of target compounds, rather they provided a significant advantage over the conventional GC-MS/MS methods, which lack sensitivity and repeatability. Strategies for minimizing losses in recovery of these compounds during sample preparation included cryogenic comminution, extraction with acidified ethyl acetate or acetonitrile, and dilution of the final extract with acidified water prior to LC-MS/MS analysis. The method performance complied with the SANTE/11813/2017 guidelines, with recoveries in the range of 70-120% at the LOQ of 0.01 mg/kg across the tested matrices at various pHs. The efficiency of the method was reflected in its precision (RSDs < 10%) for incurred residues.
本文报道了一种改进的液相色谱串联质谱法,用于测定水果和蔬菜中残留的克菌丹(+四氢邻苯二甲酰亚胺)、灭菌丹、福美双(+邻苯二甲酰亚胺)和乙菌利。优化的电喷雾电离参数(高锥气流和低脱溶剂温度)并没有导致目标化合物的降解,而是相对于缺乏灵敏度和重现性的传统 GC-MS/MS 方法具有显著优势。在样品制备过程中,为最大限度减少这些化合物回收率损失而采取的策略包括低温粉碎、酸化乙酸乙酯或乙腈提取,以及在 LC-MS/MS 分析前用酸化水稀释最终提取物。该方法的性能符合 SANTE/11813/2017 指南的要求,在不同 pH 值的各种测试基质中,LOQ 为 0.01 mg/kg 时,回收率在 70-120%范围内。该方法的效率还反映在其对实际残留的精密度(RSDs<10%)上。