Cloud Point Extraction Coupled with Ultrasonic-Assisted Back-Extraction for the HPLC-MS Determination of 1H-Triazoles in Foods

IF 2.6 3区农林科学 Q2 FOOD SCIENCE & TECHNOLOGY

Food Analytical Methods Pub Date : 2024-06-08 DOI:10.1007/s12161-024-02642-5

Veronika Yu. Moshkovska, Viktoriia O. Klovak, Valentyna M. Levchyk, Volodymyr O. Doroschuk

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Abstract

A method for the determination of tebuconazole, triadimefon, triadimenol, propiconazole, and diniconazole fungicide in vegetables, fruits, and sprouts of wheat and corn by high-performance liquid chromatography coupled to mass detection with cloud point extraction by phases of nonionic surfactant Triton X-114 was developed. The factors influencing the concentration of nonionic surfactant, medium acidity, equilibrium temperature, holding time of solutions in a water bath, and time and speed of centrifugation on extraction parameters were optimized. The complete extraction of analytes into the 0.2% (w/v) Triton X-114 phase occurs in the 2.0–9.0 pH range, provided that the analytes exist in hydrophobic electroneutral molecular forms that effectively transfer to the surfactant-rich phase of the nonionic surfactant at a temperature of 50 °C. The required time for the complete formation of the surfactant-rich phase is more than 15 min when centrifuging solutions at 4000 rpm for 12 min. The developed fungicide determination method is characterized by the limit of detection (3σ) of 0.4–0.8 ng∙mL⁻¹, the limit of quantitation (10σ) of 1.4–2.5 ng∙mL⁻¹, and a working range of 1.4–200 ng∙mL⁻¹. The developed method was applied to the determination of tebuconazole and triadimenol in beets, grapes, and sprouts of wheat and corn after their treatment with industrial fungicide preparations.

Graphical Abstract

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云点萃取与超声辅助反萃取相结合用于 HPLC-MS 检测食品中的 1H- 三唑类化合物

建立了高效液相色谱-质量检测-非离子表面活性剂Triton X-114浊点萃取测定蔬菜、水果、小麦和玉米芽菜中戊唑醇、三唑酮、三唑醇、丙环唑和二环唑杀菌剂的方法。优化了非离子表面活性剂浓度、介质酸度、平衡温度、溶液在水浴中的保温时间以及离心时间和速度对萃取参数的影响因素。在 pH 值为 2.0-9.0 的范围内，分析物可以完全萃取到 0.2%（w/v）的 Triton X-114 相中，前提是分析物以疏水性电中性分子形式存在，并能在 50 ℃ 的温度下有效转移到非离子表面活性剂的富表面活性剂相中。在 4000 rpm 转速下离心 12 分钟，富表面活性剂相完全形成所需的时间超过 15 分钟。所建立的杀菌剂测定方法的特点是检出限（3σ）为 0.4-0.8 ng∙mL-1，定量限（10σ）为 1.4-2.5 ng∙mL-1，工作范围为 1.4-200 ng∙mL-1。所建立的方法适用于甜菜、葡萄、小麦和玉米芽中经工业杀菌剂处理后的戊唑醇和三唑醇的测定。图解摘要

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来源期刊

Food Analytical Methods 农林科学-食品科技

CiteScore

6.00

自引率

3.40%

发文量

244

审稿时长

3.1 months

期刊介绍： Food Analytical Methods publishes original articles, review articles, and notes on novel and/or state-of-the-art analytical methods or issues to be solved, as well as significant improvements or interesting applications to existing methods. These include analytical technology and methodology for food microbial contaminants, food chemistry and toxicology, food quality, food authenticity and food traceability. The journal covers fundamental and specific aspects of the development, optimization, and practical implementation in routine laboratories, and validation of food analytical methods for the monitoring of food safety and quality.