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Determination of β(2)-Agonist Residues in Fermented Ham Using UHPLC-MS/MS after Enzymatic Digestion and Sulfonic Resin Solid Phase Purification

β(2)-agonists are a class of synthetic sympathomimetic drugs with acute poisoning effects if consumed as residues in foods. To improve the efficiency of sample preparation and to overcome matrix-dependent signal suppression in the quantitative analysis of four β(2)-agonists (clenbuterol, ractopamine...

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Autores principales: Cai, Chenggang, Xiang, Yannan, Tian, Siyi, Hu, Zhongce, Hu, Zhengyan, Ma, Bingjie, Wu, Pinggu
Formato: Online Artículo Texto
Lenguaje:English
Publicado: MDPI 2023
Materias:
Acceso en línea:https://www.ncbi.nlm.nih.gov/pmc/articles/PMC10004211/
https://www.ncbi.nlm.nih.gov/pubmed/36903285
http://dx.doi.org/10.3390/molecules28052039
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author Cai, Chenggang
Xiang, Yannan
Tian, Siyi
Hu, Zhongce
Hu, Zhengyan
Ma, Bingjie
Wu, Pinggu
author_facet Cai, Chenggang
Xiang, Yannan
Tian, Siyi
Hu, Zhongce
Hu, Zhengyan
Ma, Bingjie
Wu, Pinggu
author_sort Cai, Chenggang
collection PubMed
description β(2)-agonists are a class of synthetic sympathomimetic drugs with acute poisoning effects if consumed as residues in foods. To improve the efficiency of sample preparation and to overcome matrix-dependent signal suppression in the quantitative analysis of four β(2)-agonists (clenbuterol, ractopamine, salbutamol, and terbutaline) residues in fermented ham, an enzyme digestion coupled cation exchange purification method for sample preparation was established using ultra-high performance liquid chromatography and tandem mass spectrometry (UHPLC-MS/MS). Enzymatic digests were subject to cleanup treatment on three different solid phase extraction (SPE) columns and a polymer-based strong cation resin (SCR) cartridge containing sulfonic resin was found to be optimal compared with silica-based sulfonic acid and polymer sulfonic acid resins based SPEs. The analytes were investigated over the linear range of 0.5 to 10.0 μg/kg with recovery rates of 76.0–102.0%, and a relative standard deviation of 1.8–13.3% (n = 6). The limit of detection (LOD) and the limit of quantification (LOQ) were 0.1 μg/kg and 0.3 μg/kg, respectively. This newly developed method was applied to the detection of β(2)-agonist residues in 50 commercial ham products and only one sample was found to contain β(2)-agonist residues (clenbuterol at 15.2 µg/kg).
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spelling pubmed-100042112023-03-11 Determination of β(2)-Agonist Residues in Fermented Ham Using UHPLC-MS/MS after Enzymatic Digestion and Sulfonic Resin Solid Phase Purification Cai, Chenggang Xiang, Yannan Tian, Siyi Hu, Zhongce Hu, Zhengyan Ma, Bingjie Wu, Pinggu Molecules Article β(2)-agonists are a class of synthetic sympathomimetic drugs with acute poisoning effects if consumed as residues in foods. To improve the efficiency of sample preparation and to overcome matrix-dependent signal suppression in the quantitative analysis of four β(2)-agonists (clenbuterol, ractopamine, salbutamol, and terbutaline) residues in fermented ham, an enzyme digestion coupled cation exchange purification method for sample preparation was established using ultra-high performance liquid chromatography and tandem mass spectrometry (UHPLC-MS/MS). Enzymatic digests were subject to cleanup treatment on three different solid phase extraction (SPE) columns and a polymer-based strong cation resin (SCR) cartridge containing sulfonic resin was found to be optimal compared with silica-based sulfonic acid and polymer sulfonic acid resins based SPEs. The analytes were investigated over the linear range of 0.5 to 10.0 μg/kg with recovery rates of 76.0–102.0%, and a relative standard deviation of 1.8–13.3% (n = 6). The limit of detection (LOD) and the limit of quantification (LOQ) were 0.1 μg/kg and 0.3 μg/kg, respectively. This newly developed method was applied to the detection of β(2)-agonist residues in 50 commercial ham products and only one sample was found to contain β(2)-agonist residues (clenbuterol at 15.2 µg/kg). MDPI 2023-02-21 /pmc/articles/PMC10004211/ /pubmed/36903285 http://dx.doi.org/10.3390/molecules28052039 Text en © 2023 by the authors. https://creativecommons.org/licenses/by/4.0/Licensee MDPI, Basel, Switzerland. This article is an open access article distributed under the terms and conditions of the Creative Commons Attribution (CC BY) license (https://creativecommons.org/licenses/by/4.0/).
spellingShingle Article
Cai, Chenggang
Xiang, Yannan
Tian, Siyi
Hu, Zhongce
Hu, Zhengyan
Ma, Bingjie
Wu, Pinggu
Determination of β(2)-Agonist Residues in Fermented Ham Using UHPLC-MS/MS after Enzymatic Digestion and Sulfonic Resin Solid Phase Purification
title Determination of β(2)-Agonist Residues in Fermented Ham Using UHPLC-MS/MS after Enzymatic Digestion and Sulfonic Resin Solid Phase Purification
title_full Determination of β(2)-Agonist Residues in Fermented Ham Using UHPLC-MS/MS after Enzymatic Digestion and Sulfonic Resin Solid Phase Purification
title_fullStr Determination of β(2)-Agonist Residues in Fermented Ham Using UHPLC-MS/MS after Enzymatic Digestion and Sulfonic Resin Solid Phase Purification
title_full_unstemmed Determination of β(2)-Agonist Residues in Fermented Ham Using UHPLC-MS/MS after Enzymatic Digestion and Sulfonic Resin Solid Phase Purification
title_short Determination of β(2)-Agonist Residues in Fermented Ham Using UHPLC-MS/MS after Enzymatic Digestion and Sulfonic Resin Solid Phase Purification
title_sort determination of β(2)-agonist residues in fermented ham using uhplc-ms/ms after enzymatic digestion and sulfonic resin solid phase purification
topic Article
url https://www.ncbi.nlm.nih.gov/pmc/articles/PMC10004211/
https://www.ncbi.nlm.nih.gov/pubmed/36903285
http://dx.doi.org/10.3390/molecules28052039
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