Simultaneous Determination of 12 Toxic Alkaloids in Urine and Gastric Juice Using Liquid Chromatography-Electrospray Ionization Tandem Mass Spectrometry
A new method has been established for the rapid and simultaneous analysis of 12 alkaloids,thermopsine,retrorsine,anisodamine,gelsemine,gramine,harmine,emetine,sanguinarine,evodiamine,rutaecarpine,wilforine and wilforgine in urine and gastric juice samples.The conditions of extraction,chromatography and mass spectrometry were optimized,and the matrix effects and fragmentation mechanism of the alkaloids were also examined.The samples were first treated with Na 2 B 4 O 7-NaOH buffer solution(pH 9.6),then extracted by ethyl acetate twice.After evaporation,the residues were reconstituted in methanol,from which 5 μL was used for detecting by liquid chromatography-electrospray ionization tandem mass spectrometry in positive ionization mode(ESI +).The linear range was 5-200 μg/L for emetine and sanguinarine,0.5-200 μg/ L for harmine and 1-200 μg / L for other alkaloids.The mean recoveries ranged from 61.0% to 119.1% in urine samples expect thermopsine and anisodamine,and 61.0% to 110.2% in gastric juice samples.The relative standard deviations(RSDs) were less than 15%,and the limits of detection(LOD) and quantification(LOQ) varied from 0.1 to 0.5 μg/L and 0.5 to 5 μg/L.The method,proved to be rapid,sensitive and easy to handle,was suitable for the determination of trace alkaloids in urine and gastric juice samples of poisonous patients.