Detection of beta-blockers in human urine by GC-MS-MS-EI: perspectives for the antidoping control

Amendola, Luca; Molaioni, Francesco; Botrè, Francesco

doi:10.1016/s0731-7085(00)00271-5

Cited by 56 publications

(23 citation statements)

References 16 publications

(10 reference statements)

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“…Several gas chromatographic (Quaglio et al, 1993;Black et al, 1996;Hartonen and Riekkola, 1996;Amendola et al, 2000) and liquid chromatographic (Naidong et al, 2002;Maurer et al, 2004;do Carmo Borges et al, 2005;Josefsson and Sabanovic, 2006;Keski-Rahkonen et al, 2007;Li et al, 2007;Ding et al, 2007;Fanali et al, 2007) methods coupled to mass spectrometry, including tandem mass spectrometry (MS-MS), have been developed in order to determine the levels of acebutolol, labetalol, metoprolol and propranolol in biological samples. These methods utilized liquid-liquid extraction (LLE; Amendola et al, 2000;do Carmo Borges et al, 2005;KeskiRahkonen et al, 2007;Li et al, 2007) or off-line solidphase extraction (SPE; Quaglio et al, 1993;Black et al, 1996;Hartonen and Riekkola, 1996;Naidong et al, 2002;Maurer et al, 2004;Josefsson and Sabanovic, 2006) for specimen preparation and concentration prior to chromatography.…”

Section: Introductionmentioning

confidence: 99%

“…These methods utilized liquid-liquid extraction (LLE; Amendola et al, 2000;do Carmo Borges et al, 2005;KeskiRahkonen et al, 2007;Li et al, 2007) or off-line solidphase extraction (SPE; Quaglio et al, 1993;Black et al, 1996;Hartonen and Riekkola, 1996;Naidong et al, 2002;Maurer et al, 2004;Josefsson and Sabanovic, 2006) for specimen preparation and concentration prior to chromatography. However, LLE and off-line SPE methods are laborious and time-consuming.…”

Section: Introductionmentioning

confidence: 99%

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Simultaneous determination of β‐blockers in human plasma using liquid chromatography–tandem mass spectrometry

Umezawa

Lee

Arima

et al. 2008

Biomedical Chromatography

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A detailed procedure for the analysis of four beta-blockers, acebutolol, labetalol, metoprolol and propranolol, in human plasma by high-performance liquid chromatography (LC)-tandem mass spectrometry (MS-MS) using an MSpak GF column, which enables direct injection of crude plasma samples, is presented. Protein and/or macromolecule matrix compounds were eluted first from the column, while the drugs were retained on the polymer stationary phase of the MSpak GF column. The analytes retained on the column were then eluted into an acetonitrile-rich mobile phase using a gradient separation technique. All drugs showed base peak ions due to [M + H]+ ions by LC-MS with positive ion electrospray ionization, and the product ions were produced from each [M + H]+ ion by LC-MS-MS. Quantification was performed by selected reaction monitoring. The recoveries of the four beta-blockers spiked into plasma were 73.5-89.9%. The regression equations for all compounds showed excellent linearity in the range 10-1000 ng/mL of plasma, with the exception of propranolol (10-800 ng/mL). The limits of detection and quantification for each drug were 1-3 and 10 ng/mL, respectively, of plasma. The intra- and inter-day coefficients of variation for all drugs in plasma were not greater than 10.9%.

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Section: Introductionmentioning

confidence: 99%

Section: Introductionmentioning

confidence: 99%

Simultaneous determination of β‐blockers in human plasma using liquid chromatography–tandem mass spectrometry

Umezawa

Lee

Arima

et al. 2008

Biomedical Chromatography

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“…The screening analysis of b-blockers in doping control has been preferably done by gas chromatography-mass spectrometry (GC-MS) after derivatization [2,3]. More recently, the use of GC/MS/MS [4] and LC/MS/MS [5] has improved the selectivity and sensitivity of the method for screening b-blocker agents in the urine. However, such expansive material is available only in a few laboratories.…”

Section: Introductionmentioning

confidence: 99%

Simultaneous determination of thirteen β-blockers and one metabolite by gradient high-performance liquid chromatography with photodiode-array UV detection

Delamoye

Duverneuil²,

Paraire³

et al. 2004

Forensic Science International

124

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“…6,7 However, the sensitivity of these methods was limited. The most widely used were chromatographic techniques, such as gas chromatography (GC), 8,9 high-performance liquid chromatography (HPLC) [10][11][12][13][14][15][16][17] and urtra-performance liquid chromatography (UPLC). 18 Among them, expensive columns and costly apparatus were needed, and the analysis time was relatively long.…”

Section: Introductionmentioning

confidence: 99%

Determination of Atenolol and Metoprolol by Capillary Electrophoresis with Tris(2,2′-bipyridyl)ruthenium(II) Electrochemiluminescence Detection

et al. 2007

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Atenolol (AT) and metoprolol (ME) are antihypertensive drugs that belong to the family of selective β(1)-adrenergic receptor antagonists (β-blockers), which are widely used in the treatment of hypertension, angina pectoris, cardiac arrhythmias and myocardial infarction. 1 Due to their sedative effect, they are also used as doping agents in sports. An overdose of β-blockers may lead to bradycardia, hypotension, aggravation of cardiac failure, bronchospasm, hypoglycemia, and fatigue.2 Therefore, it is necessary to develop a sensitive and simple analytical method to determine β-blockers in many fields, including doping control, forensic analysis, toxicology and pharmacokinetic study.As a consequence of the widespread use of AT and ME, several analytical techniques have been developed for their determination in recent years, including spectrophotometry [3][4][5] and differential pulse voltammetry. 6,7 However, the sensitivity of these methods was limited. The most widely used were chromatographic techniques, such as gas chromatography (GC), 8,9 high-performance liquid chromatography (HPLC) [10][11][12][13][14][15][16][17] and urtra-performance liquid chromatography (UPLC). 18 Among them, expensive columns and costly apparatus were needed, and the analysis time was relatively long.The capillary electrophoresis (CE) technique has been developed for over 20 years, and has become a mature and wellestablished analytical tool. CE is characterized as a powerful separation technique because of its high efficiency, relatively short analysis time, and low sample and reagent consumption. As an alternative and complementary technique to HPLC for routine analysis, CE-UV has been used for AT and ME analysis. 19-22Because of the small sample volume being assayed, this method has encountered the problem of poor sensitivity, which has limited its application in practice. He et al. 23 developed an on-line ion-exchange preconcentration method for improving the detection sensitivity of CE-UV. The proposed method enhanced the detection sensitivity of CE-UV by about 5000 times for metoprolol compared with the normal electrokinetic injection.However, the preparation of a preconcentration column was complex for a general laboratory. Thus, it is very important to develop a simple and sensitive method to detect AT and ME.Electrochemiluminescence (also called electrogenerated chemiluminescence) is a means of converting electrical energy into radiative energy. 24 It has been proved to be a powerful analytical tool that combines the simplicity of electrochemistry and the inherent sensitivity and the wide linear range of the chemiluminescence method. 25Among the ECL systems, tris(2,2′-bipyridyl)ruthenium(II) Ru(bpy)3 2+ -based ECL is the most valuable in fundamental studies and applications because of its stability and capability of undergoing ECL at room temperature in aqueous solutions and its regenerating during the ECL process. 26Since the first report of Ru(bpy)3 2+ ECL in 1972, 27 Ru(bpy)3 2+ ECL as a sensitive detection method has been...

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Detection of beta-blockers in human urine by GC-MS-MS-EI: perspectives for the antidoping control

Cited by 56 publications

References 16 publications

Simultaneous determination of β‐blockers in human plasma using liquid chromatography–tandem mass spectrometry

Simultaneous determination of β‐blockers in human plasma using liquid chromatography–tandem mass spectrometry

Simultaneous determination of thirteen β-blockers and one metabolite by gradient high-performance liquid chromatography with photodiode-array UV detection

Determination of Atenolol and Metoprolol by Capillary Electrophoresis with Tris(2,2′-bipyridyl)ruthenium(II) Electrochemiluminescence Detection

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