An automated on-line solid-phase extraction (SPE) combined with LC–MS/MS method was developed for determination of deoxynivalenol (DON), 3-acetyl-DON and 15-acetyl-DON in corn flour and wheat flour samples. The extraction solvent of the samples was injected into the automated on-line SPE system to remove matrix interference. After washing step, the targets were eluted from the SPE cartridge into liquid chromatography (LC) column. Several SPE parameters including injection volume, elution volume and eluting flow rate were assessed and optimized. Method validation was evaluated and good linearity was obtained (R² > 99%) with the limit of detection of 0.1–0.2 μg/kg. Recoveries were evaluated in spiked corn flour and wheat flour samples at three concentrations and the values ranged from 86.5% to 99.7%. The benefit of the present method with automated on-line SPE system is the ability to inject directly pure extracts into LC–MS/MS, offering faster analyses and improving analysis efficiency.

开发了一种自动在线固相萃取 (SPE) 结合 LC-MS/MS 方法，用于测定玉米粉和小麦粉样品中的脱氧雪腐镰刀菌烯醇 (DON)、3-乙酰-DON 和 15-乙酰-DON。将样品的萃取溶剂注入自动在线 SPE 系统以去除基质干扰。洗涤步骤后，目标物从 SPE 小柱中洗脱到液相色谱 (LC) 柱中。对包括进样体积、洗脱体积和洗脱流速在内的几个 SPE 参数进行了评估和优化。评估了方法验证并获得了良好的线性 (R ² > 99%)，检测限为 0.1–0.2 μg/kg。对三种浓度的加标玉米粉和小麦粉样品的回收率进行了评估，回收率范围为 86.5% 至 99.7%。本方法与自动化在线 SPE 系统的优势在于能够将纯提取物直接注入 LC-MS/MS，从而提供更快的分析并提高分析效率。