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Titel:
Auteur:
Verschenen in: Analytical letters
Paginering: Jaargang 40 (2007) nr. 4 pagina's 737-746
Jaar: 2007-01
Inhoud: A rapid, sensitive, and selective high-performance liquid chromatography-tandem mass spectrometric method (HPLC-MS-MS) for the determination of coumatetralyl in human serum using warfarin as an internal standard has been developed and validated. Coumatetralyl and the internal standard were extracted from the human serum samples by liquid-liquid extraction with ethyl acetate, followed by separation on a XDB C18 reversed-phase column (150 mm×2.1 mm i.d., 5 µm) using a mobile phase consisting of acetic acid-ammonium acetate (5 mmol/L, pH=4.5)/methanol (20:80, v/v) at a constant flow rate of 0.40 mL/min. Coumatetralyl and the internal standard were ionized by negative ion pneumatically assisted electrospray and detected in the multiple-reaction monitoring mode using precursor→product ion combinations at m/z 291→247 and 307→161, respectively. The calibration curve was linear (r2=0.9945) in the concentration range of 0.5∼100.0 ng/mL, with a lower limit of quantification of 0.5 ng/mL in human serum. Intra- and inter-day relative standard deviations were less than 6.3 and 11.0%, respectively. The mean extraction recovery was 87.9% for coumatetralyl and 90.1% for the internal standard. This method is found to be able to determine trace coumatetralyl in human serum and can be used for the diagnosis of poisoned human beings.
Uitgever: Taylor & Francis
Bronbestand: Elektronische Wetenschappelijke Tijdschriften
 
 

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