Deep Eutectic Solvent-Based Dispersive Liquid–Liquid Microextraction Coupled with LC-MS/MS for the Analysis of Two Ochratoxins in Capsicum

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, b...

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Main Authors: Hongbo Yang, Jin Li, Jianfei Mao, Chan Xu, Jieyu Song, Feng Xie
Format: Article
Language:English
Published: MDPI AG 2023-11-01
Series:Molecules
Subjects:
Online Access:https://www.mdpi.com/1420-3049/28/22/7634
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author Hongbo Yang
Jin Li
Jianfei Mao
Chan Xu
Jieyu Song
Feng Xie
author_facet Hongbo Yang
Jin Li
Jianfei Mao
Chan Xu
Jieyu Song
Feng Xie
author_sort Hongbo Yang
collection DOAJ
description 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<sup>2</sup>) 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.
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spelling doaj.art-cafc121c14314e22bf8321665e2865e02023-11-24T14:58:30ZengMDPI AGMolecules1420-30492023-11-012822763410.3390/molecules28227634Deep Eutectic Solvent-Based Dispersive Liquid–Liquid Microextraction Coupled with LC-MS/MS for the Analysis of Two Ochratoxins in CapsicumHongbo Yang0Jin Li1Jianfei Mao2Chan Xu3Jieyu Song4Feng Xie5School of Public Health, The Key Laboratory of Environmental Pollution Monitoring and Disease Control, Ministry of Education, Guizhou Medical University, Guiyang 561113, ChinaSchool of Public Health, The Key Laboratory of Environmental Pollution Monitoring and Disease Control, Ministry of Education, Guizhou Medical University, Guiyang 561113, ChinaCollege of Chemistry, Sichuan University, Chengdu 610064, ChinaSchool of Public Health, The Key Laboratory of Environmental Pollution Monitoring and Disease Control, Ministry of Education, Guizhou Medical University, Guiyang 561113, ChinaSchool of Public Health, The Key Laboratory of Environmental Pollution Monitoring and Disease Control, Ministry of Education, Guizhou Medical University, Guiyang 561113, ChinaSchool of Public Health, The Key Laboratory of Environmental Pollution Monitoring and Disease Control, Ministry of Education, Guizhou Medical University, Guiyang 561113, ChinaOchratoxins, 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<sup>2</sup>) 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.https://www.mdpi.com/1420-3049/28/22/7634deep eutectic solventdispersive liquid–liquid microextractionochratoxinscapsicumgreen analytical chemistry
spellingShingle Hongbo Yang
Jin Li
Jianfei Mao
Chan Xu
Jieyu Song
Feng Xie
Deep Eutectic Solvent-Based Dispersive Liquid–Liquid Microextraction Coupled with LC-MS/MS for the Analysis of Two Ochratoxins in Capsicum
Molecules
deep eutectic solvent
dispersive liquid–liquid microextraction
ochratoxins
capsicum
green analytical chemistry
title Deep Eutectic Solvent-Based Dispersive Liquid–Liquid Microextraction Coupled with LC-MS/MS for the Analysis of Two Ochratoxins in Capsicum
title_full Deep Eutectic Solvent-Based Dispersive Liquid–Liquid Microextraction Coupled with LC-MS/MS for the Analysis of Two Ochratoxins in Capsicum
title_fullStr Deep Eutectic Solvent-Based Dispersive Liquid–Liquid Microextraction Coupled with LC-MS/MS for the Analysis of Two Ochratoxins in Capsicum
title_full_unstemmed Deep Eutectic Solvent-Based Dispersive Liquid–Liquid Microextraction Coupled with LC-MS/MS for the Analysis of Two Ochratoxins in Capsicum
title_short Deep Eutectic Solvent-Based Dispersive Liquid–Liquid Microextraction Coupled with LC-MS/MS for the Analysis of Two Ochratoxins in Capsicum
title_sort deep eutectic solvent based dispersive liquid liquid microextraction coupled with lc ms ms for the analysis of two ochratoxins in capsicum
topic deep eutectic solvent
dispersive liquid–liquid microextraction
ochratoxins
capsicum
green analytical chemistry
url https://www.mdpi.com/1420-3049/28/22/7634
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