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Abstract
A rapid method has been developed to analyse CP 47, 497 in human urine. Urine samples were diluted with water:acetonitrile (90:10, v/v) and sample aliquots were analysed by triple quadrupole tandem mass spectrometry with a runtime of 5 min. Multiple reaction monitoring (MRM) as survey scan was performed. The method was validated in urine, according to an in-house validation protocol based on the criteria defined in Commission Decision 2002/657/EC. Three MRM transitions were monitored. The decision limit (CCα) was 0.01μg mL⁻¹ and for the detection capability a (CCβ) value of 0.02 μg mL⁻¹ was obtained. The measurement uncertainty of the method was 21%. Fortifying human urine samples (n=18) in three separate assays, show the accuracy of the method to be between 95 and 96%. The precision of the method, expressed as RSD values for the within-lab reproducibility at the three levels of fortification (0.1, 0.15 and 0.2 μg mL⁻¹) was less than 10% respectively. The method proved to be simple, robust and time efficient. To the best of our knowledge there are no LC-MS methods for the determination of CP 47, 497 with validation data in urine.
Source: A method for C... [J Chromatogr B Analyt Technol Biomed Life Sci. 2011] - PubMed - NCBI
A rapid method has been developed to analyse CP 47, 497 in human urine. Urine samples were diluted with water:acetonitrile (90:10, v/v) and sample aliquots were analysed by triple quadrupole tandem mass spectrometry with a runtime of 5 min. Multiple reaction monitoring (MRM) as survey scan was performed. The method was validated in urine, according to an in-house validation protocol based on the criteria defined in Commission Decision 2002/657/EC. Three MRM transitions were monitored. The decision limit (CCα) was 0.01μg mL⁻¹ and for the detection capability a (CCβ) value of 0.02 μg mL⁻¹ was obtained. The measurement uncertainty of the method was 21%. Fortifying human urine samples (n=18) in three separate assays, show the accuracy of the method to be between 95 and 96%. The precision of the method, expressed as RSD values for the within-lab reproducibility at the three levels of fortification (0.1, 0.15 and 0.2 μg mL⁻¹) was less than 10% respectively. The method proved to be simple, robust and time efficient. To the best of our knowledge there are no LC-MS methods for the determination of CP 47, 497 with validation data in urine.
Source: A method for C... [J Chromatogr B Analyt Technol Biomed Life Sci. 2011] - PubMed - NCBI
