Development of a liquid chromatography–tandem mass spectrometry method for the determination of Grayanotoxins in rat blood and its application to toxicokinetic study

Solid phase extraction Quantitative Analysis
DOI: 10.1002/bmc.3190 Publication Date: 2014-04-30T07:34:19Z
ABSTRACT
A sensitive and specific high-performance liquid chromatography-tandem mass spectrometry (LC-MS/MS) method was developed for the determination of Grayanotoxin I (GTX I) III III) in rat whole blood. Grayanotoxins (GTXs) clindamycin as internal standard (IS) were extracted from blood via solid-phase extraction using PEP cartridges. Chromatographic separation analytes achieved on a Kinetex C18 (100 × 2.1 mm, 2.6 µm) reversed-phase column gradient elution with mobile phase 1% acetic acid water methanol at flow rate 0.2 mL/min. Electrospray ionization operated positive ion mode multiple reaction monitoring. The calibration curves obtained linear over concentration range 1-100 ng/mL lower limit quantification 1 GTXs. relative deviation intra-day inter-day precision below 6.8% accuracy ranged 94.8 to 106.6%. stable stability studies. validated successfully applied toxicokinetic study GTXs rats first time after oral administration 11.52 mg/kg mad honey 0.35 GTX III, respectively.
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