A sensitive and robust liquid chromatography-tandem mass spectrometric (LC-MS/MS)\nmethod was developed and validated for the determination of nimbolide in mouse serum.\nExemestane was used as the internal standard (IS). Here, we employed acetonitrile-based protein\nprecipitation (PPT) for serum sample preparation, and performed chromatographic separation using\nan ODS Hypersil C18 column (100 mm Ã? 2.1 mm, 5...) with gradient elution (0.1% formic acid\nin water vs 100% acetonitrile). The run time was 6 min. Instrumental analysis was performed by\nelectrospray ionization tandem mass spectrometry (ESI-MS/MS) in the multiple-reaction monitoring\n(MRM) under positive mode. A good linear calibration was achieved in the 5â??1000 ng/mL range.\nThe intra- and inter-day precisions for nimbolide were ............... respectively. Intra-day\naccuracy ranged from 96.9â??109.3%, while inter-day accuracy ranged from 94.3â??110.2%. The matrix\neffect of nimbolide, detected but consistent at low and high concentrations, do not affect linearity of\nstandard curve. In conclusion, we have developed and validated a sensitive analytical method for\ndetermination of a novel natural compound nimbolide in mouse serum, and it has been successfully\napplied to our preclinical study in investigating the pharmacokinetic properties of nimbolide,\nwhich could greatly facilitate the preclinical development of the promising lead compound for\nanticancer therapy.
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