Determination of bongkrekic acid in plasma of food poisoning patients by liquid chromatography-tandem mass spectrometry / 预防医学

ABSTRACT

Objective@#To quickly determine bongkrekic acid（BKA）in plasma qualitatively and quantitatively by liquid chromatography-tandem mass spectrometry（LC-MS/MS）,and to provide technical support for etiological identification of food poisoning events.@*Methods@#The plasma sample was protein precipitated with acetonitrile,diluted with water and purified with anion exchange solid phase extraction cartridge of PAX. The sample extract was separated by an XBridgeTM BEH C18 chromatographic column. Gradient elution was conducted with the mobile phase of 0.01 %（v/v）ammonia and methanol. Then BKA was detected by LC-MS/MS. @*Results@#The equation of linear regression was y=16 509x+3 134.3. Good linear relationship was obtained for BKA at a range from 1 to 400 ng/mL in plasma,with the correlation coefficient of 0.999 3. The limit of detection（LOD）was 0.5 ng/mL and the limit of quantitation（LOQ）was 1 ng/mL. The average recoveries were 76.0%-96.7% with relative standard deviations（RSDs,n=6）of 5.2%-12.8% at three spiking levels of 1（LOQ）,10（10 times of LOQ）and 200 ng/mL（medium of linear range）. The concentrations of BKA in plasma obtained from two patients suffering from food poisoning were 394 and 92.3 ng/mL. @*Conclusion@#The optimized sample pretreatment and chromatographic separation conditions can achieve rapid,accurate,qualitative and quantitative analysis of BKA in plasma.