1.Determination of Triptolide and Wilforlide A in Biological Samples by LC-MS/MS
Journal of Forensic Medicine 2015;(6):445-449,453
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.
2.Simultaneous Screening for 45 Poisonous Alkaloids in Blood by LC-MS/MS
Jinxiao ZHAI ; Min SHEN ; Wei LIU
Journal of Forensic Medicine 2015;(1):28-33
Objective To develop a liquid chromatography-tandem mass spectrometry (LC-MS/MS) screen-ing method for 45 poisonous alkaloids in blood. Methods Identification was based on the compound’s retention time and two precursor-to-production transitions. The method involved a liquid-liquid extraction (LLE) followed by LC-MS/MS with multiple-reaction monitoring (MRM). When 1 mL of blood was ex-tracted with diethyl ether at pH=9.2 with SKF525A as the internal standard, the target compounds were an-alyzed with LC-MS/MS in the positive ionization mode. Results The target alkaloids had good linearity (r>0.995 1), both the intra-day precision and inter-day precision being less than 14.77%. The limits of detection ranged from 0.05 to 25 ng/mL in blood. Conclusion The method is selective and sensitive in detecting poisonous alkaloids with a total running time of 12 minutes; therefore it was successfully ap-plied to some actual cases of suspected alkaloids poisoning.