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- Li, He, et al.
(författare)
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Quantitative analysis of valiolamine through pre-column derivatization with phenylisocyanate using high-performance liquid chromatography with UV detection : Selection of reagent, identification of derivative and optimization of derivatization conditions
- 2009
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Ingår i: Journal of Pharmaceutical and Biomedical Analysis. - : Elsevier. - 0731-7085 .- 1873-264X. ; 49:4, s. 957-963
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Tidskriftsartikel (refereegranskat)abstract
- This report describes the improved quantitative determination of valiolamine in a medium for microbial culture using high-performance liquid chromatography with UV detection. Valiolamine aqueous solution was dried, dissolved in dimethyl sulfoxide and derivatization performances of phenylisocyanate (PHI), 1-fluoro-2,4-dinitrobenznene and 1-naphthylisothiocyanate were compared in the presence of triethylamine. The PHI was chosen as the most suitable derivatization reagent and the valiolamine-PHI derivative was identified by thin-layer chromatography and electrospray ionization mass spectrometry. The derivative eluted at 10.5 min on a reverse-phase column using a mobile phase composed of 10% acetonitrile in water containing 0.5 mM sodium octyl sulfate (pH 3.0), at a column flow rate of 1.0 mL/min with UV detection at 240 nm. The optimum conditions for derivatization were a reaction temperature of 30 degrees C, reaction time of 30 min, and PHI concentration higher than 33.6 mM. Calibration curves were linear in the range of 0.99-19.95 microg/mL for the standard solutions and 24.9-99.7 microg/mL for the spiked sample. The proposed method was validated and proven to be selective, accurate and precise and suitable for the quantitative analysis of valiolamine in medium for microbial cultures.
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