Determination of amine-containing phosphonic acids and amino acids as dansyl derivatives

Conditions are selected for the analytical separation of (N-phosphonomethyl glycine), products of its microbiological conversion, glutamic acid, and alanine as dansyl derivatives using reversed-phase HPLC: column (250 × 4.6 mm) ReproSil-PAH EPA; mobile phase, methanol + 20 mM CH₃COONa (pH 5.1) (20: 80); rate of mobile phase, 1 mL/min; working detector wavelength, 330 nm. The duration of separation is 35 min. The lower limits of the analytical range (in ng) for dansyl derivatives are as follows: glyphosate, 8.2; aminomethyl phosphonic acid, 24.2; glutamic acid, 9.4; alanine, 12.6: glycine, 17.7; and sarcosine, 19.3. The TLC study of dansyl derivatives of amino acids was performed on sorbfil plates PTSH-P-V using two-dimensional chromatography in the systems ethyl acetate-isopropanol-24% aqueous ammonia (45: 35: 20) in the first direction and chloroform-methanol-acetic acid (25: 5: 1) in the second one. For determining phosphonic acids (glyphosate and aminomethyl phosphonic acid), a version of one-dimensional chromatography with the sequential use of two systems, chloroform-methanol-acetic acid (25: 5: 0.2) and ethanol-24% aqueous ammonia (7: 3), was proposed.     

Determination of Diketopiperazine Alkaloids of the Roquefortine Group by UV Spectroscopy, Thin-Layer Chromatography, and High-Performance Liquid Chromatography

Electronic absorption spectra and the chromatographic retention of six alkaloids from the roquefortine group under conditions of thin-layer chromatography and high-performance liquid chromatography were examined. The applicability of these techniques to the identification of diketopiperazine alkaloids in culture liquid extracts was demonstrated using the fungusPenicillium chrysogenumVKM F-1987 as an example.