超高效液相色谱-串联质谱法测定便携式水样中多类农药的 SPE 化学计量优化。
Chemometric Optimization of SPE for the Determination of Multiclass Pesticides in Portable Water Samples by UHPLC-MS/MS.
机构信息
Environmental Pollution Control Laboratory, Chemistry Department, Aristotle University of Thessaloniki, Thessaloniki, 54124, Greece.
Laboratory of Pharmaceutical Analysis, Department of Pharmacy, Aristotle University of Thessaloniki, Thessaloniki, 54124, Greece.
出版信息
Bull Environ Contam Toxicol. 2024 Mar 9;112(3):48. doi: 10.1007/s00128-024-03873-2.
This study aimed on the development of a SPE-UHPLC-MS/MS method for the simultaneous determination of pesticide residues in drinking water samples. A chemometric approach was applied to optimize the efficiency of the SPE pretreatment procedure. This study involved (i) the application of a Full Factorial Design for the screening of the significant factors, (ii) the application of a Central Composite Design for the determination of the optimal conditions and (iii) the evaluation and validation of the significance of the statistically proposed models. Oasis HLB cartridges were used for the extraction. The optimum sample volume was 300 mL and the elution solvent 3 mL of the mixture of methanol:ethylacetate 70:30 v/v. The method was validated according to the international guidelines. Recoveries were ranged from 63 to 116% and the detection limits were between 0.1 and 1.5 pg mL. The validated method could be used in routine analysis for pesticides screening.
本研究旨在开发一种 SPE-UHPLC-MS/MS 方法，用于同时测定饮用水样品中的农药残留。应用化学计量学方法优化 SPE 预处理程序的效率。本研究包括：（i）应用全因子设计筛选显著因素，（ii）应用中心组合设计确定最佳条件，（iii）评估和验证统计学提出模型的显著性。Oasis HLB 萃取小柱用于萃取。最佳样品体积为 300mL，洗脱溶剂为甲醇：乙酸乙酯 70:30（v/v）的混合液 3mL。该方法按照国际准则进行了验证。回收率在 63%至 116%之间，检测限在 0.1 至 1.5pg/mL 之间。验证后的方法可用于常规分析中农药的筛选。
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