Separation of D- and L-DOPA as their L-leucine derivatives by reversed-phase HPLC

Summary The separation and quantitation of D-DOPA as an impurity in L-DOPA is described. The method involves formation of the diastereomeric derivatives of DOPA with tert-butoxycarbonyl-L-leucine hydroxysuccinimide ester. Separation of the diastereomers was performed by reversed-phase liquid chromatography on LiChrosorb RP-18 and acetonitrile-phosphate buffer with addition of N,N-dimethyloctylamine as the mobile phase. The reproducibility of the method was 5.9% (relative standard deviation) at D-DOPA levels of 0.5% in L-DOPA drug substance.     

The analysis of nitrate in environmental samples by reversed-phase HPLC

A method is presented for the analysis of nitrate in natural waters and waste water by high-performance liquid chromatography (HPLC) with a reversed-phase octadecyl column, aqueous phosphoric acid/dihydrogen phosphate mobile phase, and UV detector. The optimum nitrate concentration is 0.3 to 3 mg/L as N with linear detector response below 3 mg/L. The detection limit is 0.007 mg/L. Relative standard deviations in the optimum range are consistently less than one percent. Several potential interferences have been investigated; nitrite and organic chromophores are resolved from nitrate and do not interfere. Hexavalent chromium and sulfate are slight positive interferences, negligible at typical environmental concentrations. The method produces results in agreement with the accepted chromotropic acid method except in samples from eutrophic lakes, for which evidence is presented indicating that the chromotropic acid is inaccurate.     

Synthesis of 6-nitro-4-sulfanyl-1H-indole derivatives from 2,4,6-trinitrotoluene

The synthesis of 6-nitro-4-sulfanyl-1H-indoles from 2,4,6-trinitrotoluene (TNT) is described. The first step is the nucleophilic substitution of an ortho-nitro group with a thiol to give the corresponding sulfide. The latter were transformed into the corresponding enamines upon treatment with dimethylformamide dimethyl acetal (DMF DMA). The enamines were converted into the indoles applying the Batcho–Leimgruber synthetic protocol.     

Determination of nitrite and nitrate in Venice lagoon water by ion interaction reversed-phase liquid chromatography

Ion interaction reversed-phase liquid chromatography with octylammonium orthophosphate as the interacting reagent and a reversed-phase C₁₈ column was applied to the identification and determination of nitrite and nitrate in Venice lagoon water. Interference by the high chloride concentration was systematically studied and the results obtained with different column packings were compared. With spectrophotometric detection at 230 nm, nitrite at 0.005 mg 1^?1 can be detected and determined even in the presence of 0.70 M chloride. The dependence of the retention time of nitrite on the chloride concentration was studied for two reversed-phase columns with different packings. Concentrations of 0.30 ± 0.05 mg 1^?1 of nitrite and 0.20 ± 0.05 mg 1^?1 of nitrate were found in Venice lagoon water.     

Solid-state structural properties of 2,4,6-trimethoxybenzene derivatives, determined directly from powder X-ray diffraction data in conjunction with other techniques

Structural properties of 2,4,6-trimethoxybenzaldehyde, 2,4,6-trimethoxybenzyl alcohol and 2,4,6-trimethoxyacetophenone have been determined directly from powder X-ray diffraction data, using the direct-space Genetic Algorithm (GA) technique for structure solution followed by Rietveld refinement. Structural similarities and contrasts within this family of materials are elucidated. The work illustrates the value of utilizing information from other sources, including spectroscopic data and computational techniques, as a means of augmenting the structural knowledge established from the powder X-ray diffraction data.     

Electrochemical determination of nitrite and nitrate by pneumatoamperometry

Nitrite in aqueous solution is reduced to nitric oxide with hydroquinone in pH 2 phosphate buffer. The nitric oxide is swept with nitrogen to an anodically polarized membrane-covered platinum electrode, where it is oxidized to nitrate. The resulting current is linearly related to nitrite concentration in the original solution from the detection limit of 18 nmol to 5 μmol of nitrite. Nitrate is subsequently determined similarly after reduction to nitric oxide with hydroquinone in 50% sulfuric acid containing ammonium molybdate catalyst. The linear range is from the detection limit of 40 nmol to 10 μmol of nitrate.     

Interaction of baddeleyite with sodium nitrate and nitrite

Features of baddeleiyte concentrate decomposition by interaction with sodium nitrate and nitrite were researched as well as those of hydrolytic and acid decomposition of resulting cakes.     

Determination of nitrate and nitrite with ascorbic acid

A direct titrimetric procedure has been developed for the determination of nitrate and nitrite with ascorbic acid in 9-12M phosphoric acid medium. Ferroin, N-phenylanthranilic acid, barium diphenylamine sulphonate and diphenylbenzidene can be used as the indicator. The method has also been applied for the assay of nitrate in fertilizers.     

Determination of nitrate and nitrite in mixtures with a nitrate ion electrode

A rapid method for the determination of nitrate and nitrite ions is described. The potential of a mixture of nitrate and nitrite was measured with a nitrate ion selective electrode. The nitrite in the mixture is then oxidized to nitrate with permanganate in acid solution, and the potential of the oxidized solution is also measured with the electrode. The fundamental equations for the response of the nitrate ion electrode to nitrate ion in the presence of interfering ions were used, and a new equation was developed for calculating the original nitrate concentration of the mixture. The absolute errors for solutions of known concentrations (2.5–100 p.p.m. each) were 1.8 p.p.m. nitrate and 2 p.p.m. nitrite. When the results are calculated by computer, five determinations can be performed in 30 min. The method was applied to the determination of the oxides of nitrogen in cigarette smoke as nitrite and nitrate after dissolution in basic solution.     

毛细管电泳紫外检测分析氨基酸-铜配合物

用六甲基二硅胺烷对石英毛细管进行硅烷化处理,在铜离子-庚基磺酸盐-乙酸缓冲体系中,于254nm处紫外检测分析了氨基酸。考察了各种条件对检测灵敏度和溶质迁移的影响。在合适条件下,五种氨基酸得到基线分离。     

Direct determination of N-nitrosodiethanolamine in triethanolamine with HPLC, ion-exchange chromatography and UV-detection

Summary The difference in the pK-values and chemical structure of N-nitrosodiethanolamine and triethanolamine in connection with a clear UV-maximum at 235 nm make possible a direct determination of N-nitrosodiethanolamine in triethanolamine up to 10 ng/ml possible when using an eluent of high optical transparency and a separating column with a high selectivity and reduced internal diameter. Linearity, reproducibility and accuracy meet the requirements to be fulfilled by trace-analytical methods.     

Ultra-rapid analysis of nitrate and nitrite by capillary electrophoresis

Rapid analysis of nitrate and nitrite by capillary electrophoresis (CE) has been limited by the ions' very similar electrophoretic mobilities. With a pKa of 3.15, the mobility of nitrite can be selectively reduced using a low pH buffer in CE. A much shorter capillary can be used and separation voltages can be increased. With this method, nitrate and nitrite are separated in just over 10 s. This is roughly 20 times faster than current separation methods. Direct UV detection at 214 nm was employed and offered sub microM detection limits. Total analysis time (pre-rinse, injection, and separation) was less than 1 min, making this method ideal for high-throughput analysis.     

Reactions ofβ-chloroethyl derivatives of tricoordinated phosphorus acids with 1-nitro-1-propene

Conclusions The reactions of the-chloroethyl derivatives of trivalent phosphorus acids proceed via an ionic intermediate, which, depending on the experimental conditions, is stabilized in the direction of ring closure to give an adduct with a pentacovalent phosphorus atom and the formation of the corresponding unsaturated and (-methyl--nitroethyl)phosphoryl compounds. The liberated-chloroethyl nitrite functions as an oxidizing agent of the starting-chloroethyl derivatives of trivalent phosphorus acids.Translated from Izvestiya Akademii Nauk SSSR, Seriya Khimicheskaya, No. 6, pp. 1398–1401, June, 1978.The authors thank É. I. Gol'dfarb for taking the³¹P–{¹H} NMDR spectra.