RESUMEN
Objective To determ inate triptolide and wilforlide A in biological sam ples by liquid chrom atog-raphy-tandemmass spectrom etry (LC-M S/MS)method and to verify themethod. Methods A fter 0.4mLblood, urine or 0.4 g hepatic tissues with internal standard were extracted by ethyl acetate, they were separated on a A llure PFP Propyl (100mm ×2.1mm , 5μm ) with amobile phase ofmethanol-20mm ol/Lammonium acetate using gradient elution. Formass spectrom etric detection, electrospray ionization (E SI+) in positivemode was elected and the data was collected usingmultiple-reactionmonitoring (M R M ). Results The linearity was good (r>0.995 0) and the lim it of detection was 2 ng/m Lor 2 ng/g for triptolide and wilforlide A . The recovery was 61.08% -102.98% . The intra-day and inter-day precision was less than 12.58% for each biological sam ple, and the accuracy was 90.61%-105.80%. Conclusion Thismethod is sim ple, convenient and good selective, and could be applied to analysis of triptolide and wilforlide A in different biological sam ples. A nd themethodmay provide technical support for forensicmedicine identification, clinical diagnosis and treatm ent of tripterygium wilfordii Hook. f. poisoning.
RESUMEN
Objective To establish the m ethod to analyze γ-hydroxybutyric acid (GHB ) and its precursors 1,4-butanediol (1,4-B D ) and gam m a-butyrolactone (GBL) in urine through LC-M S/M S and provide evi-dence for related cases. Methods GHB-d6 and M O R-d3 were used as the internal standard. The urine sam ple w as separated by LC after protein precipitation w ith m ethanol. The electrospray ion source w as for ionization. E ach com pound w as detected through m ultiple-reaction m onitoring (M R M ) m ode. Results The lim its of detection of GHB and its precursors 1,4-B D and GBLwere 0.1, 0.1 and 2μg/m L. The accuracy w as 87.6% -98.1% . The intra-day and inter-day precisions were less than 15% and m atrix ef-fects were higher than 80% . Conclusion The m ethod is high sensitive, sim ple, rapid, specific and w ith high reliability. This study has provided technical support and basic data for forensic cases involving GHB .