Analysis of Patulin in Apple Products Marketed in Belgium: Intra-Laboratory Validation Study and Occurrence

Apple and apple derivatives (e.g., juices, puree) are the most important foodstuffs contaminated with patulin (PAT) in the human diet. To routinely monitor these foodstuffs and ensure that the PAT levels are below the maximum permitted levels, a method using liquid chromatography combined with tande...

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Main Authors: Emmanuel K. Tangni, Julien Masquelier, Els Van Hoeck
Format: Article
Language:English
Published: MDPI AG 2023-05-01
Series:Toxins
Subjects:
Online Access:https://www.mdpi.com/2072-6651/15/6/368
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author Emmanuel K. Tangni
Julien Masquelier
Els Van Hoeck
author_facet Emmanuel K. Tangni
Julien Masquelier
Els Van Hoeck
author_sort Emmanuel K. Tangni
collection DOAJ
description Apple and apple derivatives (e.g., juices, puree) are the most important foodstuffs contaminated with patulin (PAT) in the human diet. To routinely monitor these foodstuffs and ensure that the PAT levels are below the maximum permitted levels, a method using liquid chromatography combined with tandem mass spectrometry (LC-MS/MS) has been developed. Afterwards, the method was successfully validated, reaching quantification limits of 1.2 μg/L for apple juice and cider, and 2.1 μg/kg for puree. Recovery experiments were performed with samples fortified with PAT in the range of 25–75 μg/L for juice/cider and 25–75 μg/kg for puree. The results show overall average recovery rates of 85% (RSD<sub>r</sub> = 13.1%) and 86% (RSD<sub>r</sub> = 2.6%) with maximum extended uncertainty (U<sub>max</sub>, k = 2) of 34 and 35% for apple juice/cider and puree, respectively. Next, the validated method was applied to 103 juices, 42 purees and 10 ciders purchased on the Belgian market in 2021. PAT was not found in the cider samples, but it was present in 54.4% of the tested apple juices (up to 191.1 μg/L) and 7.1% of the puree samples (up to 35.9 μg/kg). When comparing the results to the maximum levels set by Regulation EC n° 1881/2006 (i.e., 50 μg/L for juices and 25 μg/kg for puree for adults, and 10 μg/kg for infants and young children), exceedances were observed in five apple juices and one puree sample, for infants and young children. Using these data, a potential risk assessment for consumers can be suggested, and it is found that the quality of apple juices and purees sold in Belgium needs further regular surveillance.
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spelling doaj.art-f56b32892f7b477495c9cae21cb6f6822023-11-18T12:55:24ZengMDPI AGToxins2072-66512023-05-0115636810.3390/toxins15060368Analysis of Patulin in Apple Products Marketed in Belgium: Intra-Laboratory Validation Study and OccurrenceEmmanuel K. Tangni0Julien Masquelier1Els Van Hoeck2Sciensano, Chemical and Physical Health Risks, Organic Contaminants and Additives, Toxins Unit, Leuvensesteenweg 17, 3080 Tervuren, BelgiumSciensano, Chemical and Physical Health Risks, Organic Contaminants and Additives, Toxins Unit, Leuvensesteenweg 17, 3080 Tervuren, BelgiumSciensano, Chemical and Physical Health Risks, Organic Contaminants and Additives, Toxins Unit, Leuvensesteenweg 17, 3080 Tervuren, BelgiumApple and apple derivatives (e.g., juices, puree) are the most important foodstuffs contaminated with patulin (PAT) in the human diet. To routinely monitor these foodstuffs and ensure that the PAT levels are below the maximum permitted levels, a method using liquid chromatography combined with tandem mass spectrometry (LC-MS/MS) has been developed. Afterwards, the method was successfully validated, reaching quantification limits of 1.2 μg/L for apple juice and cider, and 2.1 μg/kg for puree. Recovery experiments were performed with samples fortified with PAT in the range of 25–75 μg/L for juice/cider and 25–75 μg/kg for puree. The results show overall average recovery rates of 85% (RSD<sub>r</sub> = 13.1%) and 86% (RSD<sub>r</sub> = 2.6%) with maximum extended uncertainty (U<sub>max</sub>, k = 2) of 34 and 35% for apple juice/cider and puree, respectively. Next, the validated method was applied to 103 juices, 42 purees and 10 ciders purchased on the Belgian market in 2021. PAT was not found in the cider samples, but it was present in 54.4% of the tested apple juices (up to 191.1 μg/L) and 7.1% of the puree samples (up to 35.9 μg/kg). When comparing the results to the maximum levels set by Regulation EC n° 1881/2006 (i.e., 50 μg/L for juices and 25 μg/kg for puree for adults, and 10 μg/kg for infants and young children), exceedances were observed in five apple juices and one puree sample, for infants and young children. Using these data, a potential risk assessment for consumers can be suggested, and it is found that the quality of apple juices and purees sold in Belgium needs further regular surveillance.https://www.mdpi.com/2072-6651/15/6/368mycotoxinspatulinapplejuicespureeBelgium
spellingShingle Emmanuel K. Tangni
Julien Masquelier
Els Van Hoeck
Analysis of Patulin in Apple Products Marketed in Belgium: Intra-Laboratory Validation Study and Occurrence
Toxins
mycotoxins
patulin
apple
juices
puree
Belgium
title Analysis of Patulin in Apple Products Marketed in Belgium: Intra-Laboratory Validation Study and Occurrence
title_full Analysis of Patulin in Apple Products Marketed in Belgium: Intra-Laboratory Validation Study and Occurrence
title_fullStr Analysis of Patulin in Apple Products Marketed in Belgium: Intra-Laboratory Validation Study and Occurrence
title_full_unstemmed Analysis of Patulin in Apple Products Marketed in Belgium: Intra-Laboratory Validation Study and Occurrence
title_short Analysis of Patulin in Apple Products Marketed in Belgium: Intra-Laboratory Validation Study and Occurrence
title_sort analysis of patulin in apple products marketed in belgium intra laboratory validation study and occurrence
topic mycotoxins
patulin
apple
juices
puree
Belgium
url https://www.mdpi.com/2072-6651/15/6/368
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AT julienmasquelier analysisofpatulininappleproductsmarketedinbelgiumintralaboratoryvalidationstudyandoccurrence
AT elsvanhoeck analysisofpatulininappleproductsmarketedinbelgiumintralaboratoryvalidationstudyandoccurrence