ABSTRACT
High-resolution gas chromatography (HRGC) and gas chromatography/mass spectrometry (GC/MS) are the techniques of choice to determine the retention indices of more than 200 organic acids as their trimethylsilyl (TMS) or oxime-trimethylsilyl derivatives. Several types of apolar and semipolar fused-silica capillary columns (OV-1, SE-52, and OV-1701), used to analyze and separate organic acids isolated from urine samples, are evaluated.
Subject(s)
Acids/urine , Adult , Child, Preschool , Chromatography, Gas , Flame Ionization , Humans , InfantABSTRACT
A GLC method for the specific identification and quantitation of iproiazid, a potent monamine oxidase inhibitor drug, is described. The free drug isolated from urine samples by two-phase extraction reinforced with salting out. Identification and quantitative determination at the microgram level are done on aliquots of the chloroform extract by GLC, using the 2-butyl analog as an internal standard. Iproniazid and potentially interfering compounds present in the extracts are also identified by GLC-mass spectrometry and TLC for supporting evidence of the GLC method's specificity.
Subject(s)
Iproniazid/urine , Aged , Chromatography, Gas , Chromatography, Thin Layer , Female , Humans , Iproniazid/therapeutic use , Male , Mass Spectrometry , Mental Disorders/drug therapy , Middle Aged , Time FactorsABSTRACT
Analytically packed columns prepared with Versamid-930, Versamid-900, XE-60, and OV-225 as stationary phases were examined for quantitative gas-liquid chromatography of the potent monamine oxydase inhibitor (MAOI) drugs iproniazid and iproclozide. With the aid of chemically related substances as internal standards, response ratios were determined and linearities calculated by regression analysis. Using the 2-butyl analogs of compounds all four column systems permit quantitation of iproniazid and iproclozide with a percent standard deviation sigmaK of about 1% or less.
Subject(s)
Chromatography, Gas , Glycolates/analysis , Iproniazid/analysis , Monoamine Oxidase Inhibitors/analysis , Chromatography, Liquid , Hydrazines/analysis , MethodsABSTRACT
As a result of a comparative study performed on thirteen liquid phases an improved set of four analytically packed columns, i.e., Versamid-900, Versamid-930, XE-60, and OV-225 is withheld for successful gas chromatography of iproniazid and iproclozide. Retention data in terms of adjusted retention times and relative retentions, using structurally related compounds as reference, are reported. An evaluation of gas chromatographic performance of proposed columns is described.
Subject(s)
Chromatography, Gas , Glycolates/analysis , Monoamine Oxidase Inhibitors/analysis , Chromatography, Liquid , Hydrazines/analysis , Methods , Microchemistry , Time FactorsABSTRACT
The presence of p-chlorophenoxyacetamide was detected in the urine of man receiving iproclozide [1-(p-chlorophenoxyacetyl)-2-isopropylhydrazine]. This new metabolite was identified by combined gas-liquid chromatography-mass spectrometry and by comparison with the synthetic compound. An appropriate procedure for the extraction and quantitation of p-chlorophenoxyacetamide by gas-liquid chromatography on a 5% OV-225-packed column with the 2-butyl analog of iproclozide as an internal standard, has been developed. After 20- and 50-mg single dose oral administrations of iproclozide, 5.2 and 8.3% were slowly excreted in urine as p-chlorophenoxyacetamide within 30.5 and 36 hr. respectively. After 20-mg oral intakes by psychiatric patients, the 24-hr urinary excretion of p-chlorophenoxyacetamide amounted to about 2-4% of the iproclozide dose administered.
Subject(s)
Acetamides/urine , Glycolates/metabolism , Monoamine Oxidase Inhibitors/metabolism , Adult , Chromatography, Gas , Humans , Hydrazines/metabolism , Male , Mass SpectrometryABSTRACT
Seven solvent systems for the thin-layer chromatographic separation of hydrazidic monoamine oxidase inhibitor drugs have been developed. Detection of compounds at the microgram level was performed with the aid of thirteen spray reagents.
