1.Determination of Triptolide and Wilforlide A in Biological Samples by LC-MS/MS.
Journal of Forensic Medicine 2015;31(6):445-453
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.
Chromatography, High Pressure Liquid
;
Diterpenes/urine*
;
Epoxy Compounds/urine*
;
Humans
;
Oleanolic Acid/urine*
;
Phenanthrenes/urine*
;
Sensitivity and Specificity
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Tandem Mass Spectrometry