Hebei Food Safety Key Laboratory, Hebei Food Inspection and Research Institute, Shijiazhuang, 050091, China.
College of Food Science and Technology, Hebei Agricultural University, Baoding, 071001, China.
Bull Environ Contam Toxicol. 2021 Aug;107(2):248-254. doi: 10.1007/s00128-020-02920-y. Epub 2020 Jun 26.
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 (R > 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.
建立了一种在线固相萃取（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。将样品的提取溶剂注入自动在线 SPE 系统，以去除基质干扰。在洗涤步骤后，目标物从 SPE 小柱中洗脱到液相色谱（LC）柱中。评估并优化了几个 SPE 参数，包括进样体积、洗脱体积和洗脱流速。对方法进行了验证，得到了良好的线性（R > 99%），检出限为 0.1-0.2μg/kg。在三个浓度下对添加的玉米粉和小麦粉样品进行了回收率评估，回收率范围为 86.5%-99.7%。本方法与自动在线 SPE 系统的优点是能够直接将纯提取物注入 LC-MS/MS，从而实现更快的分析并提高分析效率。
