Fatty acid ethyl esters (FAEE) in virgin olive oil: A shorter and full validated approach as an alternative to the EU Official Method

Raquel B. Gómez-Coca; María del Carmen Pérez-Camino; Paul Brereton; Alessandra Bendini; Tullia Gallina Toschi; Wenceslao Moreda

doi:10.1016/j.foodchem.2022.133300

Fatty acid ethyl esters (FAEE) in virgin olive oil: A shorter and full validated approach as an alternative to the EU Official Method

Raquel B. Gómez-Coca^*, María del Carmen Pérez-Camino, Paul Brereton, Alessandra Bendini, Tullia Gallina Toschi, Wenceslao Moreda

^*Corresponding author for this work

Research output: Contribution to journal › Article › peer-review

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Abstract

In this work a SPE/GC-FID method, incorporating the use of a 1-g silica cartridge, for the determination of FAEE in olive oils is presented. The procedure has been fully validated, initially ‘in-house’ and subsequently by an international validation study involving sixteen laboratories from Europe, the United States of America, and China. Key performance parameters of the method are: (1) Linearity in the 10–134 mg/kg range (R² > 0.999), (2) LOD and LOQ < 0.5 mg/kg, (3) RSD_r < 10%, (4) RSD_R < 20% (for 4 out of 5 test materials). In addition, the method has been demonstrated to provide equivalent results to the Official Method (Commission Regulation 2568/91) while providing advantages in terms of reductions in time and solvents and ease of automation. In fact, the proposed protocol requires 30 mL solvents and takes 1.5 h per determination instead of the 350 mL and 6 h needed in the UE Official Method.

Original language	English
Article number	133300
Number of pages	8
Journal	Food Chemistry
Volume	394
Early online date	24 May 2022
DOIs	https://doi.org/10.1016/j.foodchem.2022.133300
Publication status	Published - 15 Nov 2022

Bibliographical note

Funding Information:
The authors would like to thank Fera Science Ltd for providing the samples for this study. They would also like to thanks Tassos Koidis for his contribution to the pre-trial and as a technical expert on the methodology, and to Martyna Korytkowska as responsible for day to day liaison with participants and calculation of data. OLEUM “Advanced solutions for assuring the authenticity and quality of olive oil at a global scale” has received funding from the EC within the Horizon 2020 Program (2014–2020), GA no. 635690. The information expressed in this abstract reflects the authors’ views; the EC is not liable for the information contained therein. RBGC and MCPC performed the in-house validation. PB supervised the pre-trial and method performance study, and related statistical data. RBGC wrote the original draft. WM is WP4 Task Leader, AB is the WP4 Leader and TGT is the coordinator of the OLEUM Project. All authors contributed to manuscript revision, read and approved the submitted version.

Funding Information:
The authors would like to thank Fera Science Ltd for providing the samples for this study. They would also like to thanks Tassos Koidis for his contribution to the pre-trial and as a technical expert on the methodology, and to Martyna Korytkowska as responsible for day to day liaison with participants and calculation of data. OLEUM “Advanced solutions for assuring the authenticity and quality of olive oil at a global scale” has received funding from the EC within the Horizon 2020 Program (2014–2020), GA no. 635690. The information expressed in this abstract reflects the authors’ views; the EC is not liable for the information contained therein.

Publisher Copyright:
© 2022 The Author(s)

Keywords

Ethyl linoleate (PubChem CID: 5282184)
Ethyl oleate (PubChem CID: 5363269)
Ethyl palmitate (PubChem CID: 12366)
Ethyl stearate (PubChem CID: 8122)
Fatty acid ethyl esters (FAEE)
Fraud detection
Method validation
Methyl heptadecanoate (PubChem CID: 15609)
OLEUM
Olive oil
Soft deodorization

ASJC Scopus subject areas

Analytical Chemistry
Food Science

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10.1016/j.foodchem.2022.133300Licence: CC BY

Fatty acid ethyl esters (FAEE) in virgin olive oil: A shorter and full validated approach as an alternative to the EU Official Method
© 2022 The Authors. This is an open access article published under a Creative Commons Attribution License (https://creativecommons.org/licenses/by/4.0/), which permits unrestricted use, distribution and reproduction in any medium, provided the author and source are cited.
Final published version, 554 KBLicence: CC BY

Cite this

@article{c9f47a1288a24d31bbb49c5f99bcfa80,

title = "Fatty acid ethyl esters (FAEE) in virgin olive oil: A shorter and full validated approach as an alternative to the EU Official Method",

abstract = "In this work a SPE/GC-FID method, incorporating the use of a 1-g silica cartridge, for the determination of FAEE in olive oils is presented. The procedure has been fully validated, initially {\textquoteleft}in-house{\textquoteright} and subsequently by an international validation study involving sixteen laboratories from Europe, the United States of America, and China. Key performance parameters of the method are: (1) Linearity in the 10–134 mg/kg range (R2 > 0.999), (2) LOD and LOQ < 0.5 mg/kg, (3) RSDr < 10%, (4) RSDR < 20% (for 4 out of 5 test materials). In addition, the method has been demonstrated to provide equivalent results to the Official Method (Commission Regulation 2568/91) while providing advantages in terms of reductions in time and solvents and ease of automation. In fact, the proposed protocol requires 30 mL solvents and takes 1.5 h per determination instead of the 350 mL and 6 h needed in the UE Official Method.",

keywords = "Ethyl linoleate (PubChem CID: 5282184), Ethyl oleate (PubChem CID: 5363269), Ethyl palmitate (PubChem CID: 12366), Ethyl stearate (PubChem CID: 8122), Fatty acid ethyl esters (FAEE), Fraud detection, Method validation, Methyl heptadecanoate (PubChem CID: 15609), OLEUM, Olive oil, Soft deodorization",

author = "G{\'o}mez-Coca, {Raquel B.} and P{\'e}rez-Camino, {Mar{\'i}a del Carmen} and Paul Brereton and Alessandra Bendini and {Gallina Toschi}, Tullia and Wenceslao Moreda",

note = "Funding Information: The authors would like to thank Fera Science Ltd for providing the samples for this study. They would also like to thanks Tassos Koidis for his contribution to the pre-trial and as a technical expert on the methodology, and to Martyna Korytkowska as responsible for day to day liaison with participants and calculation of data. OLEUM “Advanced solutions for assuring the authenticity and quality of olive oil at a global scale” has received funding from the EC within the Horizon 2020 Program (2014–2020), GA no. 635690. The information expressed in this abstract reflects the authors{\textquoteright} views; the EC is not liable for the information contained therein. RBGC and MCPC performed the in-house validation. PB supervised the pre-trial and method performance study, and related statistical data. RBGC wrote the original draft. WM is WP4 Task Leader, AB is the WP4 Leader and TGT is the coordinator of the OLEUM Project. All authors contributed to manuscript revision, read and approved the submitted version. Funding Information: The authors would like to thank Fera Science Ltd for providing the samples for this study. They would also like to thanks Tassos Koidis for his contribution to the pre-trial and as a technical expert on the methodology, and to Martyna Korytkowska as responsible for day to day liaison with participants and calculation of data. OLEUM “Advanced solutions for assuring the authenticity and quality of olive oil at a global scale” has received funding from the EC within the Horizon 2020 Program (2014–2020), GA no. 635690. The information expressed in this abstract reflects the authors{\textquoteright} views; the EC is not liable for the information contained therein. Publisher Copyright: {\textcopyright} 2022 The Author(s)",

year = "2022",

month = nov,

day = "15",

doi = "10.1016/j.foodchem.2022.133300",

language = "English",

volume = "394",

journal = "Food Chemistry",

issn = "0308-8146",

publisher = "Elsevier Ltd",

}

TY - JOUR

T1 - Fatty acid ethyl esters (FAEE) in virgin olive oil: A shorter and full validated approach as an alternative to the EU Official Method

AU - Gómez-Coca, Raquel B.

AU - Pérez-Camino, María del Carmen

AU - Brereton, Paul

AU - Bendini, Alessandra

AU - Gallina Toschi, Tullia

AU - Moreda, Wenceslao

N1 - Funding Information: The authors would like to thank Fera Science Ltd for providing the samples for this study. They would also like to thanks Tassos Koidis for his contribution to the pre-trial and as a technical expert on the methodology, and to Martyna Korytkowska as responsible for day to day liaison with participants and calculation of data. OLEUM “Advanced solutions for assuring the authenticity and quality of olive oil at a global scale” has received funding from the EC within the Horizon 2020 Program (2014–2020), GA no. 635690. The information expressed in this abstract reflects the authors’ views; the EC is not liable for the information contained therein. RBGC and MCPC performed the in-house validation. PB supervised the pre-trial and method performance study, and related statistical data. RBGC wrote the original draft. WM is WP4 Task Leader, AB is the WP4 Leader and TGT is the coordinator of the OLEUM Project. All authors contributed to manuscript revision, read and approved the submitted version. Funding Information: The authors would like to thank Fera Science Ltd for providing the samples for this study. They would also like to thanks Tassos Koidis for his contribution to the pre-trial and as a technical expert on the methodology, and to Martyna Korytkowska as responsible for day to day liaison with participants and calculation of data. OLEUM “Advanced solutions for assuring the authenticity and quality of olive oil at a global scale” has received funding from the EC within the Horizon 2020 Program (2014–2020), GA no. 635690. The information expressed in this abstract reflects the authors’ views; the EC is not liable for the information contained therein. Publisher Copyright: © 2022 The Author(s)

PY - 2022/11/15

Y1 - 2022/11/15

N2 - In this work a SPE/GC-FID method, incorporating the use of a 1-g silica cartridge, for the determination of FAEE in olive oils is presented. The procedure has been fully validated, initially ‘in-house’ and subsequently by an international validation study involving sixteen laboratories from Europe, the United States of America, and China. Key performance parameters of the method are: (1) Linearity in the 10–134 mg/kg range (R2 > 0.999), (2) LOD and LOQ < 0.5 mg/kg, (3) RSDr < 10%, (4) RSDR < 20% (for 4 out of 5 test materials). In addition, the method has been demonstrated to provide equivalent results to the Official Method (Commission Regulation 2568/91) while providing advantages in terms of reductions in time and solvents and ease of automation. In fact, the proposed protocol requires 30 mL solvents and takes 1.5 h per determination instead of the 350 mL and 6 h needed in the UE Official Method.

AB - In this work a SPE/GC-FID method, incorporating the use of a 1-g silica cartridge, for the determination of FAEE in olive oils is presented. The procedure has been fully validated, initially ‘in-house’ and subsequently by an international validation study involving sixteen laboratories from Europe, the United States of America, and China. Key performance parameters of the method are: (1) Linearity in the 10–134 mg/kg range (R2 > 0.999), (2) LOD and LOQ < 0.5 mg/kg, (3) RSDr < 10%, (4) RSDR < 20% (for 4 out of 5 test materials). In addition, the method has been demonstrated to provide equivalent results to the Official Method (Commission Regulation 2568/91) while providing advantages in terms of reductions in time and solvents and ease of automation. In fact, the proposed protocol requires 30 mL solvents and takes 1.5 h per determination instead of the 350 mL and 6 h needed in the UE Official Method.

KW - Ethyl linoleate (PubChem CID: 5282184)

KW - Ethyl oleate (PubChem CID: 5363269)

KW - Ethyl palmitate (PubChem CID: 12366)

KW - Ethyl stearate (PubChem CID: 8122)

KW - Fatty acid ethyl esters (FAEE)

KW - Fraud detection

KW - Method validation

KW - Methyl heptadecanoate (PubChem CID: 15609)

KW - OLEUM

KW - Olive oil

KW - Soft deodorization

U2 - 10.1016/j.foodchem.2022.133300

DO - 10.1016/j.foodchem.2022.133300

M3 - Article

AN - SCOPUS:85132904058

SN - 0308-8146

VL - 394

JO - Food Chemistry

JF - Food Chemistry

M1 - 133300

ER -

Fatty acid ethyl esters (FAEE) in virgin olive oil: A shorter and full validated approach as an alternative to the EU Official Method

Abstract

Bibliographical note

Keywords

ASJC Scopus subject areas

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