Determination of Triptolide and Wilforlide A in Biological Samples by LC-MS/MS.
- Author:
Jin-xiao ZHAI
;
Wei LIU
- Publication Type:Journal Article
- MeSH:
Chromatography, High Pressure Liquid;
Diterpenes/urine*;
Epoxy Compounds/urine*;
Humans;
Oleanolic Acid/urine*;
Phenanthrenes/urine*;
Sensitivity and Specificity;
Tandem Mass Spectrometry
- From:
Journal of Forensic Medicine
2015;31(6):445-453
- CountryChina
- Language:Chinese
-
Abstract:
OBJECTIVE:To determinate triptolide and wilforlide A in biological samples by liquid chromatography-tandem mass spectrometry (LC-MS/MS) method and to verify the method.
METHODS:After 0.4 mL blood, urine or 0.4 g hepatic tissues with internal standard were extracted by ethyl acetate, they were separated on a Allure PFP Propyl (100 mm x 2.1 mm, 5 µm) with a mobile phase of methanol-20 mmol/L ammonium acetate using gradient elution. For mass spectrometric detection, electrospray ionization (ESI⁺) in positive mode was elected and the data was collected using multiple-reaction monitoring (MRM).
RESULTS:The linearity was good (r > 0.995 0) and the limit of detection was 2 ng/mL or 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 sample, and the accuracy was 90.61%-105.80%.
CONCLUSION:This method is simple, convenient and good selective, and could be applied to analysis of triptolide and wilforlide A in different biological samples. And the method may provide technical support for forensic medicine identification, clinical diagnosis and treatment of tripterygium wilfordii Hook. f. poisoning.
