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Article

Determination of β2-Agonist Residues in Fermented Ham Using UHPLC-MS/MS after Enzymatic Digestion and Sulfonic Resin Solid Phase Purification

by
Chenggang Cai
1,
Yannan Xiang
1,
Siyi Tian
1,
Zhongce Hu
2,*,
Zhengyan Hu
3,
Bingjie Ma
3 and
Pinggu Wu
3,*
1
College of Biological and Chemical Engineering, Zhejiang University of Science and Technology, Hangzhou 310023, China
2
College of Biotechnology and Bioengineering, Zhejiang University of Technology, Hangzhou 310014, China
3
Zhejiang Provincial Center for Disease Control and Prevention, Hangzhou 310051, China
*
Authors to whom correspondence should be addressed.
Molecules 2023, 28(5), 2039; https://doi.org/10.3390/molecules28052039
Submission received: 2 February 2023 / Revised: 12 February 2023 / Accepted: 20 February 2023 / Published: 21 February 2023
(This article belongs to the Special Issue Application of LC-MS/MS in Biochemistry II)
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Abstract

β2-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 β2-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 β2-agonist residues in 50 commercial ham products and only one sample was found to contain β2-agonist residues (clenbuterol at 15.2 µg/kg).
Keywords: matrix effects; β2-agonist residues; ham; solid phase extraction; UHPLC-MS/MS matrix effects; β2-agonist residues; ham; solid phase extraction; UHPLC-MS/MS

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MDPI and ACS Style

Cai, C.; Xiang, Y.; Tian, S.; Hu, Z.; Hu, Z.; Ma, B.; Wu, P. Determination of β2-Agonist Residues in Fermented Ham Using UHPLC-MS/MS after Enzymatic Digestion and Sulfonic Resin Solid Phase Purification. Molecules 2023, 28, 2039. https://doi.org/10.3390/molecules28052039

AMA Style

Cai C, Xiang Y, Tian S, Hu Z, Hu Z, Ma B, Wu P. Determination of β2-Agonist Residues in Fermented Ham Using UHPLC-MS/MS after Enzymatic Digestion and Sulfonic Resin Solid Phase Purification. Molecules. 2023; 28(5):2039. https://doi.org/10.3390/molecules28052039

Chicago/Turabian Style

Cai, Chenggang, Yannan Xiang, Siyi Tian, Zhongce Hu, Zhengyan Hu, Bingjie Ma, and Pinggu Wu. 2023. "Determination of β2-Agonist Residues in Fermented Ham Using UHPLC-MS/MS after Enzymatic Digestion and Sulfonic Resin Solid Phase Purification" Molecules 28, no. 5: 2039. https://doi.org/10.3390/molecules28052039

APA Style

Cai, C., Xiang, Y., Tian, S., Hu, Z., Hu, Z., Ma, B., & Wu, P. (2023). Determination of β2-Agonist Residues in Fermented Ham Using UHPLC-MS/MS after Enzymatic Digestion and Sulfonic Resin Solid Phase Purification. Molecules, 28(5), 2039. https://doi.org/10.3390/molecules28052039

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