Gas chromatographic analysis of xylidine isomers on heteroaromatic compounds

Summary Nicotinic acid, picolinic acid, isonicotinic acid, histidine and other amphoteric heteroaromatic compounds, uracil, thymine, isatin and other heteroaromatic compounds having imino and carbonyl groups as well as IH-benzotriazole, benzoguanamine and guanidine phosphate effectively resolved all the xylidine (dimethylaniline) isomers. Furthermore, the mixed phases of nicotinamide + p-amino-benzoic acid and melamine+barbituric acid also provided an appreciable resolution. These analyses were carried out using a support which were not treated with an alkali.     

Nucleosides as stationary phases for the separation of xylenol isomers by gas-liquid chromatography

Summary Adenosine, guanosine and inosine used as liquid phases in gas chromatography permits the separation of all six xylenol isomers.     

Separation of alkadiene-1-ol isomers by gas-liquid chromatography

Complete gas-liquid chromatographic separation of the four 10, 12-hexadecadiene-l-ol isomers using a FFAPcoated glass capillary column is described. These measurements are of importance for the analysis of pheromones from biological sources and for the control of material from stereospecific syntheses.     

Separation of xylidine isomers by micellar electrokinetic chromatography

Xylidines are important precursors for the production of dyes, drugs, and various other products. Because of the high carcinogenic nature of some xylidine isomers it becomes very essential and relevant to develop suitable analytical procedures to separate isomers as well as enhance detection at very low concentrations. Micellar electrokinetic chromatography has been standardized at various influencing parameters such as pH, ionic strength, and micelle modifiers, and the optimum conditions have been ascertained for the best separation and sensitivity of standard mixtures. The applicability of the procedure in environmental samples is studied.     

Separation behaviors of xylenol isomers by gas chromatography with helps of hydrogen bonding

Summary Xylenol isomers can be resolved on most polyols (sugars or sugar alcohols) and polyethers (polyethylene glycol or polypropylene glycol) with hydrogen-bonding interaction. They are separated on vinical polyols which have more hydroxy hydrogen than tetrol, and even on vicinal triol when its hydroxy hydrogen is acidic (stronger proton donor). The stronger is the hydrogen bonding interaction between xylenols and the liquid phase, the better is the separation of 2,4- and 2,5-xylenol, and the poorer the separation of 2,4-and 2,3-xylenol.     

Determination of toluenesulfonic acid isomers by gas chromatography

Summary A gas chromatographic method for the determination of isomeric distribution in toluenesulfonic acid samples is described. The acids are transformed into the corresponding ethyl esters by reaction with triethyl orthoformate in toluene. The reaction mixture can be injected, without further purification, into the gas chromatograph. The separation is best performed on columns containing OV-210 or polyphenyl ether (6 rings) as the stationary phase.     

Separation ofcis andtrans isomers of naturally occurring hydroxycinnamic acids by high-pressure liquid chromatography

Summary The separation of hydroxycinnamic acids has been investigated by high-pressure liquid chromatography using a micro C₁₈ bonded phase. Irradiation oftrans-ferulic and sinapic acids readily gave a mixture ofcis-trans isomers which can be also separated with the system described.     

Gas chromatographic method for the analysis of nitrochlorobenzene isomers

Summary An efficient, reproducible and rapid gas chromatographic method for the analysis of nitrochlorobenzenes has been described in this paper. The method uses FFAP as stationary phase and 3,4-dichloronitrobenzene as internal standard. The total analysis time of the method is less than 15 minutes with a coefficient of variation ranging from 0.41% to 1.19% for different levels of three isomers.     

Separation of diarylethene-based photoswitchable isomeric compounds by high-performance liquid chromatography and supercritical fluid chromatography

Diarylethene-based photoswitches have become very popular over the last few decades for potential applications in chemistry, materials science, and biotechnology due to their unique physical and chemical properties. We report the isomeric separation of a diarylethene-based photoswitchable compound using high-performance liquid chromatography. The separated isomers were characterized by ultraviolet-visible spectroscopy and mass spectrometry confirmed the isomeric nature of the compounds. The isomers were purified by preparative high-performance liquid chromatography, providing fractionated samples to study the isomers individually. A total amount of 13 mg of an isomer of interest was fractionated from a solution of 0.4 mg/ml of the isomeric mixture. Because the preparative high-performance liquid chromatographic method required large quantities of solvent, we explored the use of supercritical fluid chromatography as an alternative separation mode which, to the best of our knowledge, is the first time this technique is used to separate diarylethene-based photoswitchable compounds. Supercritical fluid chromatography provided faster analysis times while maintaining sufficient baseline resolution for the separated compounds and consuming less organic solvent in the mobile phase compared to high-performance liquid chromatography. It is proposed that the supercritical fluid chromatographic method be upscaled and used in future fractionation of the diarylethene isomeric compounds, becoming a more environmentally benign approach for compound purification.     

Purification of CIS-trimedlure isomers by high-performance liquid chromatography

Summary High-performance liquid chromatographic procedures were developed to make it possible to obtain the fourcis-trimedlure isomers (V, W, X, and Y) in pure form. Trimedlure-V and-Y were each readilt separated from the four-componentcis-trimedlure mixture through high-performance liquid chromatographic analysis on 5-μm and 3-μm silica, but trimedlure-W and-X were not adequately resolved. Chromatography of 5-μm silica of the mixtures obtained by epimerization of thetrans-trimedlure isomers, C and B₂, yielded the respective epimers, trimedlure-W and-X, in pure form.     

Gas chromatography of some prostaglandins

Summary The synthetic prostaglandin F_2α (PG_2α), used as an ovulation regulator, and abortion inducer, is contaminated with its Δ5-trans isomer. The ratio of the isomers was measured by capillary GC. The prostaglandin I₂ (PGI₂), a blood platelet aggregation inhibitor, easily decomposes to 6-ketoprostaglandin F_1α (6-keto PG_1α). Their ratio was measured by packed column GC. An unexpected, instantaneous methanol cleavage was observed during the GC analysis of the methyl ketal derivative of 6-keto PG_1α, forming a mixture of PGI₂ and Δ6-prostaglandin I₁ (Δ6-PGI₁). Presented at the 15th International Symposium on Chromatography, Nürnberg, October 1984     

High-performance liquid chromatographic analysis of dinitrobenzene isomers

Summary An efficient, reproducible and rapid high-performance liquid chromatographic method, in normal phase mode, for the analysis of the three dinitrobenzene isomers is described. The method affords good linearity for each isomer in the range 10–160 g ml^–1. The total analysis time is only 10 minutes, and the method shows an accuracy of ±1.25% with a coefficient of variation from 0.30% to 2.85% for different levels of the dinitrobenzene isomers.     

Peculiar features of sorption of positional isomers of formyl-, acetyl-, and aminopyridines in capillary gas-liquid chromatography

The GLC retention parameters of α-, β-, and γ-isomers of formyl-, acetyl-, and aminopyridines were determined on two columns with stationary phases of different polarities. The contributions of formyl, acetyl, methyl, and amino groups located in the α-, β-, and γ-positions of the ring to the retention indices were calculated. The contributions of these groups to the retention were found to depend on their positions with respect to the N atom of the ring and are the smallest for α-substituents. The difference between pyridines containing electron-withdrawing substituents and those containing electron-donating substituents is manifested as different orders of elution of α-, β-, and γ-derivatives. The distinctions between the GLC behaviors of pyridines, benzenes, and furans with the same substituents were identified. Translated fromIzvestiya Akademii Nauk. Seriya Khimicheskaya, No. 1, pp. 91–94, January, 1997.     

Retention behavior of dipeptide isomers in reversed-phase high-performance liquid chromatography

Summary The effects of eluent pH and organic modifier concentration on the capacity factor (k) and selectivity of dipeptide isomers were investigated. It has been observed that the variation in the logarithm of the capacity factor of the dipeptide isomers is linearly dependent on the organic modifier concentration (C_b), however, the selectivity is almost independent of it. Both capacity factor and selectivity were seriously affected by the pH of the eluent. Both the capacity factor and the intercept of the ln k vs. C_b plot increased with increasing van der Waals volume of the non-polar amino acid subunit of the dipeptides.     

Gas-liquid chromatographic resolution of free dichlorophenol isomers on new stationary liquid phases

Summary It is difficult to separate all the dichlorophenol isomers as free phenols by gas-liquid chromatography. However they were effectively separated on 4,4-dimethoxyazoxybenzene (liquid crystal), and all the isomers were separated appreciably well on sodium 1-naphthalenesulfonate, 2-naphthalenesulfonate and dodecylbenzenesulfonate.     

Comparison of two liquid crystals as stationary phases in capillary gas chromatography

Summary The comparative gas chromatographic behavior has been investigated for two new liquid-crystal stationary phases, 2-(3-chlorobenzyloxy)-3-hexanoxy-4-(4-chlorobenzoyloxy)-4′-(4-methylbenzoyloxy)azobenzene (denoted 3-Cl) and 2-(3-methylbenzyloxy)-3-hexanoxy-4-(4-chlorobenzoyloxy)-4′-(4-methylbenzoyloxy)azobenzene (denoted 3-CH₃). The structures of the main core of the two liquid crystals are the same but they differ by lateral aromatic branch— 3-chlorobenzyloxy and 3-methylbenzoyloxy. Their thermal properties were established by use of differential scanning calorimetry (DSC) and their chromatographic separation properties by use of glass capillary columns. Interesting analytical performance was obtained in the separation of isomeric aromatic compounds, polyaromatic compounds, volatile aroma compounds, andcis andtrans isomers. Separation efficiency was higher for 3-Cl, especially for volatile aroma compounds, light aromatic compounds, and polyaromatic compounds, although the phases were similar in otherways.     

Gas chromatography in qualitative analyses. An investigation of the oxidation of some silicones used as gas chromatographic stationary phases

Summary The on-column oxidation of apolar and polar silicones used as gas chromatographic stationary phases is investigated. Even at 225° the effects of oxidation are found to be slight. Of the materials investigated the methylphenylsilicones are the most stable.     

Separation of technical waxes by temperature-programmed packed-capillary liquid chromatography

Summary A high-melting saturated hydrocarbon wax in the carbon range C₂₈ to C₉₀, with an average molecular mass of 785, and a saponified, oxidized Fisher-Tropsch wax of average molecular mass 745 have been characterized by reversed-phase packed-capillary liquid chromatography with isocratic nonaqueous mobile phases. High-temperature injection, temperature-programming, and miniaturized evaporative light-scattering detection were successfully employed for these separations. The injection of the wax samples, of low solubility at ambient temperature, was achieved by use of a high-temperature sample-introduction device. Temperature programming was required to achieve satisfactory resolution between the numerous components of the complex was samples.