Total Fat Gravimetric Method Workflow in Portuguese Olives Using Closed-Vessel Microwave-Assisted Extraction (MAE)

A simple and rapid method for the quantitation of total fat in olive samples is designed, evaluated, and presented. This method is based on an innovative closed-vessel microwave-assisted extraction (MAE) technique. A method was designed for olives, and some figures of merits were evaluated: limit of...

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Main Authors: João Gonçalo Lourenço, Daniel Ettlin, Inês Carrero Cardoso, Jesus M. Rodilla
Format: Article
Language:English
Published: MDPI AG 2021-10-01
Series:Foods
Subjects:
Online Access:https://www.mdpi.com/2304-8158/10/10/2364
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author João Gonçalo Lourenço
Daniel Ettlin
Inês Carrero Cardoso
Jesus M. Rodilla
author_facet João Gonçalo Lourenço
Daniel Ettlin
Inês Carrero Cardoso
Jesus M. Rodilla
author_sort João Gonçalo Lourenço
collection DOAJ
description A simple and rapid method for the quantitation of total fat in olive samples is designed, evaluated, and presented. This method is based on an innovative closed-vessel microwave-assisted extraction (MAE) technique. A method was designed for olives, and some figures of merits were evaluated: limit of detection (LOD), limit of quantification (LOQ) and expanded uncertainty (U). The data obtained in these experiences show that the workflow of the MAE method in a closed container is statistically equivalent to the other two methods, showing in this case better performance indicators (LOD = 0.02%, LOQ = 0.06%, and U = 15%). In addition, it is also demonstrated that the complete MAE method workflow allows the determination of total fat in a maximum of 12 analyses simultaneously for about 100 min in each run, which is the capacity of the rotor. This is a much better productivity when compared to the traditional Soxhlet-based method. Considering the sample workflow, the closed-vessel MAE method greatly simplifies sample handling, therefore minimizing sample loss during sample preparation and reducing analysis time. When MAE is compared to NIR-based methods, the advantage comes from there being no need for any type of calibration in the sample matrix. The MAE method itself can be used to determine the reference value for NIR calibration purposes. The results obtained for CRM using MAE were equivalent to the ones shown on the certificate.
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spelling doaj.art-8a98b1b38b3e43d8aa21942a376569852023-11-22T18:14:54ZengMDPI AGFoods2304-81582021-10-011010236410.3390/foods10102364Total Fat Gravimetric Method Workflow in Portuguese Olives Using Closed-Vessel Microwave-Assisted Extraction (MAE)João Gonçalo Lourenço0Daniel Ettlin1Inês Carrero Cardoso2Jesus M. Rodilla3Departamento de Química, Universidade da Beira Interior, Rua Marquês d’Ávila e Bolama, 6200-001 Covilhã, PortugalUnicam Sistemas Analíticos, Alameda António Sérgio, 1495-132 Algés, PortugalISEC–Instituto Superior de Engenharia de Coimbra, Rua Pedro Nunes, 3030-199 Coimbra, PortugalDepartamento de Química, Universidade da Beira Interior, FibEnTech-Materiais Fibrosos e Tecnologias Ambientais, Rua Marquês d’Ávila e Bolama, 6200-001 Covilhã, PortugalA simple and rapid method for the quantitation of total fat in olive samples is designed, evaluated, and presented. This method is based on an innovative closed-vessel microwave-assisted extraction (MAE) technique. A method was designed for olives, and some figures of merits were evaluated: limit of detection (LOD), limit of quantification (LOQ) and expanded uncertainty (U). The data obtained in these experiences show that the workflow of the MAE method in a closed container is statistically equivalent to the other two methods, showing in this case better performance indicators (LOD = 0.02%, LOQ = 0.06%, and U = 15%). In addition, it is also demonstrated that the complete MAE method workflow allows the determination of total fat in a maximum of 12 analyses simultaneously for about 100 min in each run, which is the capacity of the rotor. This is a much better productivity when compared to the traditional Soxhlet-based method. Considering the sample workflow, the closed-vessel MAE method greatly simplifies sample handling, therefore minimizing sample loss during sample preparation and reducing analysis time. When MAE is compared to NIR-based methods, the advantage comes from there being no need for any type of calibration in the sample matrix. The MAE method itself can be used to determine the reference value for NIR calibration purposes. The results obtained for CRM using MAE were equivalent to the ones shown on the certificate.https://www.mdpi.com/2304-8158/10/10/2364microwave-assisted extractiontotal fatsoxhletNIRolives
spellingShingle João Gonçalo Lourenço
Daniel Ettlin
Inês Carrero Cardoso
Jesus M. Rodilla
Total Fat Gravimetric Method Workflow in Portuguese Olives Using Closed-Vessel Microwave-Assisted Extraction (MAE)
Foods
microwave-assisted extraction
total fat
soxhlet
NIR
olives
title Total Fat Gravimetric Method Workflow in Portuguese Olives Using Closed-Vessel Microwave-Assisted Extraction (MAE)
title_full Total Fat Gravimetric Method Workflow in Portuguese Olives Using Closed-Vessel Microwave-Assisted Extraction (MAE)
title_fullStr Total Fat Gravimetric Method Workflow in Portuguese Olives Using Closed-Vessel Microwave-Assisted Extraction (MAE)
title_full_unstemmed Total Fat Gravimetric Method Workflow in Portuguese Olives Using Closed-Vessel Microwave-Assisted Extraction (MAE)
title_short Total Fat Gravimetric Method Workflow in Portuguese Olives Using Closed-Vessel Microwave-Assisted Extraction (MAE)
title_sort total fat gravimetric method workflow in portuguese olives using closed vessel microwave assisted extraction mae
topic microwave-assisted extraction
total fat
soxhlet
NIR
olives
url https://www.mdpi.com/2304-8158/10/10/2364
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