Comparative analytical quantitation of clenbuterol in biological matrices using GC-MS and EIA

Abukhalaf, Imad K.; Deutsch, Daniel A. von; Parks, Bryan A.; Wineski, Larry; Paulsen, Douglas F.; Aboul‐Enein, Hassan Y.; Potter, David E.

doi:10.1002/(sici)1099-0801(200004)14:2<99::aid-bmc933>3.0.co;2-g

Cited by 35 publications

(7 citation statements)

References 26 publications

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“…For the current study, the extraction method of Wilson et al (1994) was used for sample preparation and the quantitative determination of clenbuterol (Smith, 2000). Although the method of Wilson et al (1994) has been fairly assessed as "long and tedious" (Abukhalaf et al, 2000), the method has been validated for multiple tissues (Wilson et al, 1994), can be used for quantitative analysis (Smith, 2000), has been used by regulatory agencies for surveillance purposes (Mitchell and Dunnavan, 1998), and, as demonstrated in this study, is useful for the preparation of samples for stereochemical analysis. The method was of sufficient sensitivity so that 1 ppb of clenbuterol residue could be measured (hog lung, Table 3; 7-day withdrawal; gilts).…”

Section: Discussionmentioning

confidence: 99%

Stereochemical Composition of Clenbuterol Residues in Edible Tissues of Swine

2000

J. Agric. Food Chem.

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A gas chromatography-mass spectrometry method was developed to measure the stereochemical residues of clenbuterol derivatives in edible tissues of swine. Clenbuterol present in tissue extracts was derivatized with phosgene to form clenbuterol oxazolidin-3-one, which was then separated into component enantiomers using a dimethyl beta-cyclodextrin capillary gas chromatographic column. Purified clenbuterol stereoisomers, isolated using published liquid chromatographic techniques, were used to determine stereoisomer elution order, stereoisomer racemization potential, and accuracy of the method. The stereochemical composition of clenbuterol could be measured at tissue concentrations of <2 ppb using the method. The dextrorotatory stereoisomer was the predominant clenbuterol stereoisomer present in edible tissues of hogs slaughtered after withdrawal periods of 0, 3, and 7 days, with a (+)/(-) isomer ratio of about 3:1. The prevalence of the dextrorotatory stereoisomer in edible tissues of hogs at all withdrawal periods suggests that stereoselective processes are occurring during the absorption, distribution, metabolism, and (or) excretion of clenbuterol. The effect of clenbuterol dose on its stereochemical composition in edible tissues is unknown but will be an area of further investigation.

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Section: Discussionmentioning

confidence: 99%

Stereochemical Composition of Clenbuterol Residues in Edible Tissues of Swine

2000

J. Agric. Food Chem.

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“…Clenbuterol ( Figure 1A), one of the families of β 2 -adrenergic agonists, is mainly used as a bronchodilator for the treatment of asthma and other respiratory diseases (1). However, owing to the property of enhancing muscle and decreasing fat deposition, clenbuterol was illegally used in the animal industry, and it led many poisoning incidents (2).…”

Section: Introductionmentioning

confidence: 99%

Rapid Determination of Clenbuterol in Pork by Direct Immersion Solid-Phase Microextraction Coupled with Gas Chromatography–Mass Spectrometry

Ye¹,

Wu²,

Xu³

et al. 2015

J Chromatogr Sci

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Direct immersion solid-phase microextraction (DI-SPME) coupled with gas chromatography-mass spectrometry (GC-MS) was developed for rapid analysis of clenbuterol in pork for the first time. In this work, a low-cost homemade 44 µm polydimethylsiloxane (PDMS) SPME fiber was employed to extract clenbuterol in pork. After extraction, derivatization was performed by suspending the fiber in the headspace of the 2 mL sample vial saturated with a vapor of 100 µL hexamethyldisilazane. Lastly, the fiber was directly introduced to GC-MS for analysis. All parameters that influenced absorption (extraction time), derivatization (derivatization reagent, time and temperature) and desorption (desorption time) were optimized. Under optimized conditions, the method offered a wide linear range (10-1000 ng g(-1)) and a low detection limit (3.6 ng g(-1)). Finally, the method was successfully applied in the analysis of pork from the market, and recoveries of the method for spiked pork were 97.4-105.7%. Compared with the traditional solvent extraction method, the proposed method was much cheaper and fast.

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“…Recent studies have shown that many methods can be applied for screening and identification of β 2 ‐agonists in biological samples, such as high‐performance liquid chromatography (HPLC) with ultraviolet detection (Yan et al ., , ; Blomgren et al ., ) and fluorescence detection (Hu et al ., ), liquid chromatography–tandem mass spectrometry (Shao et al, ; Dong et al, ), gas chromatography–mass spectrometry (GC‐MS; Abukhalaf et al ., ; He et al, ), enzymelinked immunoassay (Johansson and Hellenas, ; Posyniak et al ., ; Lu et al ., ), capillary electrophoresis with amperometric detection (Chen et al ., ), and electrochemical method with differential‐pulse voltammetry (Moane et al ., ). In these articles, the extraction and purification of β 2 ‐agonists from food samples was mainly performed by solid‐phase extraction (SPE; Yan et al ., ; Shao et al ., ; Dong et al ., ).…”

Section: Introductionmentioning

confidence: 99%

Combined solid‐phase microextraction and high‐performance liquid chromatography with ultroviolet detection for simultaneous analysis of clenbuterol, salbutamol and ractopamine in pig samples

Zhang

et al. 2013

Biomedical Chromatography

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A simple and sensitive method based on the combination of solid-phase microextraction (SPME) and high-performance liquid chromatography with ultroviolet detection was developed for the simultaneous determination of clenbuterol, salbutamol and ractopamine in pig samples. Parameters of the SPME procedure affecting extraction efficiency, such as the type of fiber, extraction time, extraction temperature, ion strength, pH of sample and stirring rate, were optimized. The developed method was validated according to the International Conference on Harmonization guidelines. The calibration curves were linear over a range of 0.5-50 µg/L for clenbuterol and ractopamine, and 0.2-20 µg/L for salbutamol. The limits of detection were 0.1 µg/L for clenbuterol, 0.05 µg/L for salbutamol and 0.1 μg/L for ractopamine, respectively. The averages of intra- and inter-day accuracy ranged from 79.8 to 92.4%. The intra-day and inter-day precision were below 9.6% for the three analytes. This method exhibited the advantages of simplicity, rapidity and low solvent consumption, and was suitable for the monitoring of β2 -agonists residue in pig samples.

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Comparative analytical quantitation of clenbuterol in biological matrices using GC-MS and EIA

Cited by 35 publications

References 26 publications

Stereochemical Composition of Clenbuterol Residues in Edible Tissues of Swine

Stereochemical Composition of Clenbuterol Residues in Edible Tissues of Swine

Rapid Determination of Clenbuterol in Pork by Direct Immersion Solid-Phase Microextraction Coupled with Gas Chromatography–Mass Spectrometry

Combined solid‐phase microextraction and high‐performance liquid chromatography with ultroviolet detection for simultaneous analysis of clenbuterol, salbutamol and ractopamine in pig samples

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