Simultaneous determination of aconitine and mesaconitine in urine by liquid-liquid extraction combined with ultra high performance liquid chromatography-tandem mass spectrometry
A method for simultaneous determination of the content of aconitine and mesaconitine in urine by liquid-liquid extraction combined with ultra high performance liquid chromatography-tandem mass spectrometry was established.A certain amount of extraction solvent was added to the urine sample.The upper organic phase was separated from urine by vortex and centrifugation.The extraction procedure was repeated twice and the two extracts were combined,evaporated with nitrogen gas to dryness.The residues were re-dissolved in acetonitrile.The mobile phase consisted of acetonitrile and 0.1%formic acid-2 mmol/L ammonium formate solution.The analytes were separated by an Acquity BEH C18 column with gradient elution.The compounds were identified under electrospray ionization with positive ion mode and multiple reactions monitoring mode.The analytes were qualitative analyzed by retention time and characteristic mass ion,and quantified by external standard method.The mass concentration of aconitine and mesaconitine had a good linear relationship with the chromatographic peak area in the range of 1.0-100.0 μg/L,the correlation coefficients were not less than 0.998,and the detection limit of the method was 0.01 μg/L.The average recoveries of sample spiked were 99.2%-105.4%,and the relative standard deviations of the determination results were 1.7%-4.1%(n=5).The method is sensitive and accurate,which is suitable for the detection of aconitine and mesaconitine in food poisoning patient's urine.
aconitinemesaconitineliquid-liquid extractionultra high performance liquid chromatography-tandem mass spectrometryurine
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维普
