School of Public Health, The Key Laboratory of Environmental Pollution Monitoring and Disease Control, Ministry of Education, Guizhou Medical University, Guiyang 561113, China.
College of Chemistry, Sichuan University, Chengdu 610064, China.
Molecules. 2023 Nov 16;28(22):7634. doi: 10.3390/molecules28227634.
Ochratoxins, a common class of mycotoxin in capsicum, and techniques and methods for the determination of mycotoxins in spices have been increasingly developed in recent years. An innovative and eco-friendly method of dispersive liquid-liquid microextraction (DLLME) was demonstrated in this study, based on a synthesized deep eutectic solvent (DES) combined with LC-MS/MS, for the quantification and analysis of two ochratoxins in capsicum. The DES-DLLME method parameters entail selecting the DES type (thymol:decanoic acid, molar ratio 1:1) and DES volume (100 μL). The volume of water (3 mL) and salt concentration (0 g) undergo optimization following a step-by-step approach to achieve optimal target substance extraction efficiency. The matrix effect associated with the direct detection of the target substance in capsicum was significantly reduced in this study by the addition of isotopic internal standards corresponding to the target substance. This facilitated optimal conditions wherein quantitative analysis using LC-MS/MS revealed a linear range of 0.50-250.00 µg/mL, with all two curves calibrated with internal standards showing correlation coefficients (r) greater than 0.9995. The method's limits of detection (LODs) and limits of quantification (LOQs) fell in the ranges of 0.14-0.45 μg/kg and 0.45-1.45 μg/kg, respectively. The method's spiked recoveries ranged from 81.97 to 105.17%, indicating its sensitivity and accuracy. The environmental friendliness of the technique was assessed using two green assessment tools, AGREE and complexGAPI, and the results showed that the technique was more in line with the concept of sustainable development compared to other techniques for detecting ochratoxins in capsicum. Overall, this study provides a new approach for the determination of mycotoxins in a complex food matrix such as capsicum and other spices using DES and also contributes to the application of green analytical chemistry methods in the food industry.
辣椒中的一种常见真菌毒素——赭曲霉毒素，以及测定香料中真菌毒素的技术和方法，近年来得到了越来越多的发展。本研究提出了一种基于合成深共晶溶剂（DES）结合 LC-MS/MS 的新型绿色分散液液微萃取（DLLME）方法，用于定量和分析辣椒中的两种赭曲霉毒素。DES-DLLME 方法参数涉及选择 DES 类型（麝香草酚：癸酸，摩尔比 1:1）和 DES 体积（100μL）。按照逐步优化的方法，优化水（3mL）体积和盐浓度（0g），以达到最佳目标物质萃取效率。本研究通过添加与目标物质相对应的同位素内标物，显著降低了直接检测辣椒中目标物质时的基质效应。这有利于优化条件，使用 LC-MS/MS 进行定量分析时，线性范围为 0.50-250.00µg/mL，所有两条曲线均用内标物校准，相关系数（r）均大于 0.9995。方法的检出限（LOD）和定量限（LOQ）分别为 0.14-0.45μg/kg 和 0.45-1.45μg/kg。方法的加标回收率范围为 81.97-105.17%，表明其具有较高的灵敏度和准确性。本研究使用两种绿色评估工具 AGREE 和 complexGAPI 评估了该技术的环境友好性，结果表明与其他用于检测辣椒中赭曲霉毒素的技术相比，该技术更符合可持续发展的理念。总的来说，本研究为使用 DES 测定辣椒等复杂食品基质中的真菌毒素提供了一种新方法，也为绿色分析化学方法在食品工业中的应用做出了贡献。
