Improved screening method for beta-blockers in urine using solid-phase extraction and capillary gas...

Area of Science:

• Analytical Chemistry
• Forensic Toxicology
• Pharmacology

Background:

• Beta-blockers are commonly used medications with potential for misuse in sports.
• Accurate and sensitive detection of beta-blockers in biological samples is crucial for anti-doping efforts.
• Existing screening methods may lack the required sensitivity or specificity for timely detection.

Purpose of the Study:

• To develop and validate an improved screening method for detecting beta-blockers in urine samples.
• To enhance the sensitivity and specificity of beta-blocker detection for doping control.
• To evaluate different derivatization techniques for improved chromatographic analysis.

Main Methods:

• Enzymatic hydrolysis of urine samples to release beta-blockers.
• Solid-phase extraction (SPE) for sample cleanup and concentration.
• Capillary gas chromatography-mass spectrometry (GC-MS) for separation and detection.
• Comparison of derivatization agents: trimethylsilyl-trifluoroacetyl, trifluoroacetyl, and cyclic n-butylboronate.

Main Results:

• The developed method demonstrated high specificity and sensitivity for beta-blocker detection.
• Analyte detection was achieved up to 48 hours post-administration.
• Evaluation confirmed the suitability of specific derivatization techniques for GC-MS analysis.
• Optimized SPE and hydrolysis steps improved overall method efficiency.

Conclusions:

• The proposed screening method is effective for the specific and sensitive detection of beta-blockers in urine.
• The method's ability to detect analytes up to 48 hours post-dosage is valuable for doping control.
• This approach offers a reliable tool for forensic toxicology and anti-doping laboratories.