A validated qualitative method using oleuropein as a robust biomarker to confirm ground black pepper (Piper nigrum L.) adulteration with olive (Olea europaea L.) by-products

Olive stone and olive pomace were first identified as black pepper adulterants at the end of the 19th century. Nowadays, there is a worldwide boom in olive oil consumption. The olive oil and table olive industry generate tremendous volumes of olive wastes and this is presenting fraudsters with signi...

Full description

Bibliographic Details
Main Authors: Jean-Louis Lafeuille, Maryline Brun, Stéphane Lefèvre, Clare Menezes, Ingrid Fiordaliso Candalino
Format: Article
Language:English
Published: Elsevier 2022-06-01
Series:NFS Journal
Subjects:
Online Access:http://www.sciencedirect.com/science/article/pii/S2352364622000050
_version_ 1818776336134569984
author Jean-Louis Lafeuille
Maryline Brun
Stéphane Lefèvre
Clare Menezes
Ingrid Fiordaliso Candalino
author_facet Jean-Louis Lafeuille
Maryline Brun
Stéphane Lefèvre
Clare Menezes
Ingrid Fiordaliso Candalino
author_sort Jean-Louis Lafeuille
collection DOAJ
description Olive stone and olive pomace were first identified as black pepper adulterants at the end of the 19th century. Nowadays, there is a worldwide boom in olive oil consumption. The olive oil and table olive industry generate tremendous volumes of olive wastes and this is presenting fraudsters with significant opportunities to use olive oil by-products as bulking agents in other foods such as black pepper. Despite the development of analytical methods for black pepper (Piper nigrum L.) authentication, it has been difficult to both detect and identify the specific fraudulent addition of Olea europaea L. waste by-products to this well-known spice. As such, there is a need for the development of a targeted method to address this issue. In this study, a secoiridoid phenolic biomarker of olive oil by-products, oleuropein, was identified as a target for the development of a novel analytical method, coupling ASE®) extraction and LC-MS/MS analysis for the identification of phenolic compounds as biomarkers of black pepper adulteration with olive wastes. The described operating conditions were used for the quantitation of oleuropein in olive oil by-products as well as the qualitative detection and identification of oleuropein in black pepper as a proof of the presence of olive waste addition as a bulking agent. Oleuropein was detected and quantified in all the olive oil by-product samples, even those subjected to processes such as olive-pomace extraction with hexane and sterilisation with steam heat-treatment. The method was validated for the qualitative detection of oleuropein in black pepper with selectivity and specificity values equal to 1 for 1.5% of olive pomace addition. The proposed method is simple and automated, requiring no purification step and can be applied as a rapid routine analysis to arm the industry against this potential fraud.
first_indexed 2024-12-18T11:11:19Z
format Article
id doaj.art-5208f985db27458fa7baa60c3cab7cc0
institution Directory Open Access Journal
issn 2352-3646
language English
last_indexed 2024-12-18T11:11:19Z
publishDate 2022-06-01
publisher Elsevier
record_format Article
series NFS Journal
spelling doaj.art-5208f985db27458fa7baa60c3cab7cc02022-12-21T21:09:59ZengElsevierNFS Journal2352-36462022-06-01272127A validated qualitative method using oleuropein as a robust biomarker to confirm ground black pepper (Piper nigrum L.) adulteration with olive (Olea europaea L.) by-productsJean-Louis Lafeuille0Maryline Brun1Stéphane Lefèvre2Clare Menezes3Ingrid Fiordaliso Candalino4Global Quality and Food Safety Center of Excellence, McCormick & Co., Inc., 999 avenue des Marchés, 84200 Carpentras, France; Corresponding author.Food Integrity Laboratory, Global Quality and Food Safety Center of Excellence, McCormick & Co., Inc., 999 avenue des Marchés, 84200 Carpentras, FranceFood Integrity Laboratory, Global Quality and Food Safety Center of Excellence, McCormick & Co., Inc., 999 avenue des Marchés, 84200 Carpentras, FranceGlobal Quality and Food Safety Center of Excellence, McCormick & Co., Inc., Haddenham Business Park, Pegasus Way, Haddenham Bucks HP17 8LB, UKGlobal Quality and Food Safety Center of Excellence, McCormick & Co., Inc., Viale Iotti Nilde, 50038 San Piero (FI), ItalyOlive stone and olive pomace were first identified as black pepper adulterants at the end of the 19th century. Nowadays, there is a worldwide boom in olive oil consumption. The olive oil and table olive industry generate tremendous volumes of olive wastes and this is presenting fraudsters with significant opportunities to use olive oil by-products as bulking agents in other foods such as black pepper. Despite the development of analytical methods for black pepper (Piper nigrum L.) authentication, it has been difficult to both detect and identify the specific fraudulent addition of Olea europaea L. waste by-products to this well-known spice. As such, there is a need for the development of a targeted method to address this issue. In this study, a secoiridoid phenolic biomarker of olive oil by-products, oleuropein, was identified as a target for the development of a novel analytical method, coupling ASE®) extraction and LC-MS/MS analysis for the identification of phenolic compounds as biomarkers of black pepper adulteration with olive wastes. The described operating conditions were used for the quantitation of oleuropein in olive oil by-products as well as the qualitative detection and identification of oleuropein in black pepper as a proof of the presence of olive waste addition as a bulking agent. Oleuropein was detected and quantified in all the olive oil by-product samples, even those subjected to processes such as olive-pomace extraction with hexane and sterilisation with steam heat-treatment. The method was validated for the qualitative detection of oleuropein in black pepper with selectivity and specificity values equal to 1 for 1.5% of olive pomace addition. The proposed method is simple and automated, requiring no purification step and can be applied as a rapid routine analysis to arm the industry against this potential fraud.http://www.sciencedirect.com/science/article/pii/S2352364622000050Piper nigrumBlack pepperOlea europaeaOliveOleuropeinAdulteration
spellingShingle Jean-Louis Lafeuille
Maryline Brun
Stéphane Lefèvre
Clare Menezes
Ingrid Fiordaliso Candalino
A validated qualitative method using oleuropein as a robust biomarker to confirm ground black pepper (Piper nigrum L.) adulteration with olive (Olea europaea L.) by-products
NFS Journal
Piper nigrum
Black pepper
Olea europaea
Olive
Oleuropein
Adulteration
title A validated qualitative method using oleuropein as a robust biomarker to confirm ground black pepper (Piper nigrum L.) adulteration with olive (Olea europaea L.) by-products
title_full A validated qualitative method using oleuropein as a robust biomarker to confirm ground black pepper (Piper nigrum L.) adulteration with olive (Olea europaea L.) by-products
title_fullStr A validated qualitative method using oleuropein as a robust biomarker to confirm ground black pepper (Piper nigrum L.) adulteration with olive (Olea europaea L.) by-products
title_full_unstemmed A validated qualitative method using oleuropein as a robust biomarker to confirm ground black pepper (Piper nigrum L.) adulteration with olive (Olea europaea L.) by-products
title_short A validated qualitative method using oleuropein as a robust biomarker to confirm ground black pepper (Piper nigrum L.) adulteration with olive (Olea europaea L.) by-products
title_sort validated qualitative method using oleuropein as a robust biomarker to confirm ground black pepper piper nigrum l adulteration with olive olea europaea l by products
topic Piper nigrum
Black pepper
Olea europaea
Olive
Oleuropein
Adulteration
url http://www.sciencedirect.com/science/article/pii/S2352364622000050
work_keys_str_mv AT jeanlouislafeuille avalidatedqualitativemethodusingoleuropeinasarobustbiomarkertoconfirmgroundblackpepperpipernigrumladulterationwitholiveoleaeuropaealbyproducts
AT marylinebrun avalidatedqualitativemethodusingoleuropeinasarobustbiomarkertoconfirmgroundblackpepperpipernigrumladulterationwitholiveoleaeuropaealbyproducts
AT stephanelefevre avalidatedqualitativemethodusingoleuropeinasarobustbiomarkertoconfirmgroundblackpepperpipernigrumladulterationwitholiveoleaeuropaealbyproducts
AT claremenezes avalidatedqualitativemethodusingoleuropeinasarobustbiomarkertoconfirmgroundblackpepperpipernigrumladulterationwitholiveoleaeuropaealbyproducts
AT ingridfiordalisocandalino avalidatedqualitativemethodusingoleuropeinasarobustbiomarkertoconfirmgroundblackpepperpipernigrumladulterationwitholiveoleaeuropaealbyproducts
AT jeanlouislafeuille validatedqualitativemethodusingoleuropeinasarobustbiomarkertoconfirmgroundblackpepperpipernigrumladulterationwitholiveoleaeuropaealbyproducts
AT marylinebrun validatedqualitativemethodusingoleuropeinasarobustbiomarkertoconfirmgroundblackpepperpipernigrumladulterationwitholiveoleaeuropaealbyproducts
AT stephanelefevre validatedqualitativemethodusingoleuropeinasarobustbiomarkertoconfirmgroundblackpepperpipernigrumladulterationwitholiveoleaeuropaealbyproducts
AT claremenezes validatedqualitativemethodusingoleuropeinasarobustbiomarkertoconfirmgroundblackpepperpipernigrumladulterationwitholiveoleaeuropaealbyproducts
AT ingridfiordalisocandalino validatedqualitativemethodusingoleuropeinasarobustbiomarkertoconfirmgroundblackpepperpipernigrumladulterationwitholiveoleaeuropaealbyproducts