Establishment of a Method for Analyzing the Zilpaterol Residue in Beef Using Tandem Mass Spectrometry

Chae, Young-Sik; Moon, Jin-Ah; Baek, Seung‐Hwa

doi:10.3136/fstr.20.1165

Cited by 6 publications

(2 citation statements)

References 14 publications

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“…4 Food regulation authorities such as the United States Food and Drug Administration (FDA) have therefore implemented maximum residue levels for zilpaterol in cattle meat (Table 1). Although various assays employing high-performance liquid chromatography-mass spectrometry (HPLC-MS) for the detection and quantification of zilpaterol in meat were previously published, [5][6][7][8][9][10][11] only few studies described the metabolism of zilpaterol: data from rat and cattle elimination studies suggest that most of the administered zilpaterol is excreted unchanged. 12,13 In cattle urine, deisopropyl zilpaterol represented 2.5%-5.7% of the eliminated drug, and also a sulfate conjugate of zilpaterol was detected, but the majority of zilpaterol was reported to be excreted unconjugated.…”

Section: Introductionmentioning

confidence: 99%

Determination and enantioselective separation of zilpaterol in human urine after mimicking consumption of contaminated meat using high‐performance liquid chromatography with tandem mass spectrometry techniques

Euler

Wagener

Thomas

et al. 2022

Rapid Comm Mass Spectrometry

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Rationale: The synthetic β-adrenoreceptor agonist zilpaterol is legitimately used as an animal feed supplement in selected countries due to its known effects on lipolysis and protein biosynthesis. These pharmacological characteristics of zilpaterol have contributed to its classification as doping agent in sport by the World Anti-Doping Agency. However, the use as a feed supplement can lead to residues of the drug in edible tissues and, possibly, also in the urine of consumers.Methods: To provide urinary elimination profiles of microdosed zilpaterol and to determine whether the ingestion of zilpaterol below or at the acceptable daily intake level of 0.04 μg/kg bodyweight can result in an adverse analytical finding (AAF) in doping controls, healthy volunteers were administered single or multiple oral doses of 0.5 μg or 3 μg zilpaterol to mimic ingestion of contaminated cattle meat. Urine samples were collected and analyzed using a validated high-performance liquid chromatography-electrospray ionization-tandem mass spectrometry (HPLC-ESI-MS/ MS) method and a newly developed chiral high-performance liquid chromatographyatmospheric pressure chemical ionization-tandem mass spectrometry (HPLC-APCI-MS/MS) method.Results: Urinary peak concentrations of zilpaterol were observed for all volunteers 1.5-12.5 h after ingestion, and maximum levels >5 ng/mL, which would constitute an AAF in doping controls, were found after the intake of 3 μg of zilpaterol on five consecutive days in one out of five study participants. Noteworthy, the enantiomeric ratio of excreted zilpaterol remained constant over time. Conclusion:This study provides first insights into the urinary excretion of microdosed zilpaterol. Furthermore, a method was successfully developed and applied for the separation of the zilpaterol enantiomers with mass spectrometric detection.

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Section: Introductionmentioning

confidence: 99%

Determination and enantioselective separation of zilpaterol in human urine after mimicking consumption of contaminated meat using high‐performance liquid chromatography with tandem mass spectrometry techniques

Euler

Wagener

Thomas

et al. 2022

Rapid Comm Mass Spectrometry

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“…For this reason, the use of clenbuterol (and all other β 2 -agonists in the EU and Asia, including Japan) as a growth promoter in livestock has been prohibited [1][2][3][4][5][6][7]. However, ractopamine and zilpaterol, which are also β 2 -agonists, are less toxic than clenbuterol and they are allowed as feed additives for livestock in some countries [6,[24][25][26][27]. Even in countries where the use of these β 2 -agonists is not permitted, livestock products imported from other countries may still contain β 2 -agonists.…”

Section: Introductionmentioning

confidence: 99%

Simultaneous Determination of Seven β<sub>2</sub>-Agonists in Livestock Products Using an LC-MS/MS System

Hayashi

Hamase

2022

Chromatography

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A simultaneous determination method for seven β 2 -agonists (clenbuterol, ractopamine, zilpaterol, cimaterol, isoxsuprine, salbutamol and terbutaline) was developed using liquid chromatography tandem mass spectrometry (LC-MS/MS) to evaluate their residual status in livestock products commercially available in Japan. The livestock sample was homogenized with ethyl acetate under alkaline conditions and degreased with n-hexane. The target β 2 -agonists were then purified by dispersive solid-phase extraction with C18 particles. For the LC separation, a semi-micro scale column packed with an octadecylsilica (ODS) stationary phase was employed, and gradient elution was performed for 10 min using aqueous acetonitrile containing ammonium acetate as the mobile phase solvent, where the target compounds were eluted within 5-8 min. The developed method was validated using pig muscle, a processed pork food, cattle muscle and a processed beef food, and the obtained trueness values were 60.1-103.5%. The obtained relative standard deviation (RSD) values were 1.26-8.94% (repeatability) and 1.93-10.55% (intermediate precision). In some of the imported livestock products, small but clear peaks of ractopamine were detected by the developed LC-MS/MS method, and the presence of ractopamine was further confirmed by an LC-MS/MS/MS analysis with higher selectivity.

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Determination of zilpaterol in a residue depletion study using LC-MS/MS in cattle plasma, muscle, liver and kidney

et al. 2022

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Establishment of a Method for Analyzing the Zilpaterol Residue in Beef Using Tandem Mass Spectrometry

Abstract: Establishment of an analytical method on zilpaterol (ZPT),

Cited by 6 publications

References 14 publications

Determination and enantioselective separation of zilpaterol in human urine after mimicking consumption of contaminated meat using high‐performance liquid chromatography with tandem mass spectrometry techniques

Determination and enantioselective separation of zilpaterol in human urine after mimicking consumption of contaminated meat using high‐performance liquid chromatography with tandem mass spectrometry techniques

Simultaneous Determination of Seven β<sub>2</sub>-Agonists in Livestock Products Using an LC-MS/MS System

Determination of zilpaterol in a residue depletion study using LC-MS/MS in cattle plasma, muscle, liver and kidney

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