Gas Chromatography of Urinary Kynurenine Through Decomposition by Barium Hydroxide

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Urinary kynurenine was converted into 2-aminoacetophenone by heating with barium hydroxide and was analyzed in the form of its trifluoroacetyl derivative by gas chromatography. The peak having a retention time equal to that of authentic 2-trifluoroacetylaminoacetophenone was investigated by combined gas chromatography-mass spectrometry. The procedures are shown in the following lines.<BR>Ten ml of saturated barium hydroxide and 1g of barium hy droxide powder were added to 10ml of urine sample, and the mixture was heated in a boiling water bath under ref lux for 20min. After cooling in an ice bath, 1.0ml of chloroform solution containing p-xylene-dichloride as an internal standard was added, and the solution was extracted with twice 5ml of chloroform. The combined chloroform extract was evaporated to dryness under reduced pressure, and a drop of ethylacetate and two drops of trifluoroacetic anhydride were added to the residue, and the reaction solution was injected onto the gas chromatograph.
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