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Hoffmann, R. A wiki for the life sciences where authorship matters. Nature Genetics (2008)
 
 
 
 
 

Quantitative determination of antalarmin, a novel corticotropin-releasing hormone receptor-1 antagonist, in canine plasma by HPLC-MS.

A simple and rapid method was developed for the quantitation of antalarmin from plasma using high performance liquid chromatography coupled with electrospray ionization mass spectrometry ( ESI/MS). Separation of antalarmin from interfering compounds was achieved using reversed phase chromatography on a C-8 micro-column with an isocratic mobile phase comprised of 80% acetonitrile, 20% water, and 5 mM triethylamine. Detection by ESI/MS was accomplished in positive ion mode using single ion monitoring of the protonated molecular ions of antalarmin and its (13)C2-isotopimer. The area ratio of the integrated peaks of interest in the extracted ion chromatogram was used for quantitation. The lower limit of detection was 1 picogram (pg) and the quantitation showed a linear response up to 4 nanograms loaded on column. To achieve acceptable accuracy at or around the limit of quantitation of 20 pg, a 1/x weighting was applied to the calibration data. Accuracy and precision variation for intra and inter-day validation were below the acceptable limit (15%) for pharmacokinetic studies.[1]

References

  1. Quantitative determination of antalarmin, a novel corticotropin-releasing hormone receptor-1 antagonist, in canine plasma by HPLC-MS. Fox, S.D., Roman, J.M., Cizza, G., Veenstra, T.D., Issaq, H.J. Journal of separation science. (2005) [Pubmed]
 
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