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  • P-ISSN 1225-0163
  • E-ISSN 2288-8985

Simultaneous GC/MS Analyses of Organic acids and Amino acids in Urine using TMS-TFA dervative

Analytical Science and Technology / Analytical Science and Technology, (P)1225-0163; (E)2288-8985
2006, v.19 no.1, pp.107-114

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Abstract

Early diagnosis and medical intervention are critical for the treatment of patients with metabolic disorders. A rapid analytical method was developed for simultaneous quantification of organic acids and amino acids in urine without labor-intensive pre-extraction procedure showing high sensitivity and specificity. A new method consisted of simple two-step trimethylsilyl (TMS)-trifluoroacetyl (TFA) derivatization using GC/MS-selective ion monitoring (SIM). Filter paper urine specimens were dried under nitrogen after being fortified with internal standard (tropate) in a mixture of distilled water and methanol. Methyl orange was added to the residue as indicator reagent. Silyl derivative of carboxylic functional group was followed by trifluoroacetyl derivative for amino functional group. N-methyl-N-(trimethylsilyl-trifluoroacetamide) and N-methyl-bistrifluoroacetamide were consecutively added and heated for 15-20 min at <TEX>$65^{\circ}C-70^{\circ}C$</TEX>, for TMS-TFA derivative, respectively. This reactant was analyzed by GC/MS-SIM. Linear dynamic range showed 0.001-50 mg with the detection limit of (S/N

keywords
simultaneous analysis, organic acids and amino acids, trimethylsilyl-trifluoroacetyl derivative, GC-MS


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