ABSTRACT
The performance of a strong cation exchange-type (SCX) chiral stationary phase (CSP) was evaluated with subcritical fluid chromatography (subFC) and high performance liquid chromatography (HPLC). The chromatographic conditions in subFC were optimized by changing the amount of polar organic modifier, concentration of a basic additive in the modifier, system pressure and temperature. In this way the concentration of in situ formed transient ionic species could be varied. The gradual change of the concentration of the transient buffer, i.e. gradient elution conditions in subFC, was found beneficial for separation of a mixture of racemic compounds. The strength and amount of the in situ formed buffer was estimated on the basis of comparative experiments in subSFC and HPLC.
Subject(s)
Cations/chemistry , Chromatography, High Pressure Liquid/instrumentation , Chromatography, Ion Exchange/instrumentation , Chromatography, Supercritical Fluid/instrumentation , Amines/analysis , Amines/chemistry , Amines/isolation & purification , Ammonia/chemistry , Carbonic Acid/chemistry , Chromatography, High Pressure Liquid/methods , Chromatography, Ion Exchange/methods , Chromatography, Supercritical Fluid/methods , Pressure , Stereoisomerism , TemperatureABSTRACT
We report a chiral high-performance liquid chromatographic enantioseparation method for free α-aminophosphonic, ß-aminophosphonic, and γ-aminophosphonic acids, aminohydroxyphosphonic acids, and aromatic aminophosphinic acids with different substitution patterns. Enantioseparation of these synthons was achieved by means of high-performance liquid chromatography on CHIRALPAK ZWIX(+) and ZWIX(-) (cinchona-based chiral zwitterionic ion exchangers) under polar organic chromatographic elution conditions. Mobile phase characteristics such as acid-to-base ratio, type of counterion, and solvent composition were systematically varied in order to investigate their effect on the separation performance and to achieve optimal separation conditions for the set of analytes. Under the optimized conditions, 32 of 37 racemic aminophosphonic acids studied reached baseline separation when we employed a single generic mass-spectrometry-compatible mobile phase, with reversal of the elution order when we used (+) and (-) versions of the chiral stationary phase.
Subject(s)
Amino Acids/isolation & purification , Chromatography, Ion Exchange/methods , Ion Exchange Resins/chemistry , Phosphorous Acids/isolation & purification , Quinidine/chemistry , Quinine/chemistry , Amino Acids/chemistry , Chromatography, High Pressure Liquid/methods , Cinchona/chemistry , Phosphorous Acids/chemistry , StereoisomerismABSTRACT
The performances of ionic liquid (1-hexyl-3-methylimidazolium-bis(trifluoromethylsulfonyl)imide, IL/CPE) and iron phthalocyanine (IP/CPE) modified carbon paste electrodes in electroanalytical determinations of rutin were evaluated and compared to the performance of unmodified carbon paste electrode (CPE). Cyclic voltammetry (CV), differential pulse voltammetry (DPV), differential pulse adsorptive stripping voltammetry (DPAdSV), and amperometry were used for rutin analysis. The best current responses of rutin were obtained at pH 4.0 for all tested techniques. IL/CPE electrode was found to perform best with DPAdSV technique, where a detection limit (LOD) as low as 5 nmol L(-1) of rutin was found. On the other hand, IP/CPE showed itself to be an optimum choice for DPV technique, where LOD of 80 nmol L(-1) was obtained. Analytical applicability of newly prepared electrodes was demonstrated on determination of rutin in the model samples and the extracts of buckwheat seeds. To find an optimum method for buckwheat seeds extraction, a boiling water extraction (BWE), Soxhlet extraction (SE), pressurized solvent extraction (PSE), and supercritical fluid extraction (SFE) were tested.
