Liquid chromatographic analysis and isolation of diastereoisomers obtained by an aldolization reaction

1995 ◽  
Vol 73 (10) ◽  
pp. 1733-1737 ◽  
Author(s):  
Michel Lafosse ◽  
Philippe Morin ◽  
Christophe Anceau ◽  
Gérard Coudert ◽  
Gérald Guillaumet ◽  
...  

A new route using an aldolization reaction has been investigated in order to synthesize a precursor of pilocarpin, an alkaloid having sympathomimetic properties. To study the stereoselectivity of this route and to propose a mechanism, liquid chromatography has been used to analyse and to isolate each diastereoisomer for a structural determination by NMR. To further investigate the reaction mechanism, seven different aldehydes (or ketones) were used in the aldolization reaction, producing seven different mixtures. This paper describes the improvement of LC conditions with diol- and amino-bonded silica and the nonaqueous mobile phases required for the isolation of each isomer. Keywords: diastereoisomers, pilocarpin precursor, normal phase liquid chromatography, diol- and amino-bonded silicas.

1984 ◽  
Vol 67 (4) ◽  
pp. 698-700
Author(s):  
W Jeffrey Hurst ◽  
Michael D Aleo ◽  
Robert A Martin

Abstract A method using liquid chromatography was developed for the analysis of cholesterol in milk chocolate products. The method involves saponification of the sample with methanolic KOH followed by extraction with ether. Potentially interfering components are eliminated through the use of a silica Sep-Pak cleanup step before injection. The nonaqueous reverse phase LC system consists of a C18 column and an isopropanol- hexane mobile phase with direct detection at 205 nm. Recoveries of 1, 3, and 5 mg cholesterol added to 1 g sample of milk chocolate were 88.6, 102.8, and 110.1%, respectively. Studies conducted with [4-14C]-cholesterol were undertaken to further document the accuracy of the method.


1980 ◽  
Vol 26 (10) ◽  
pp. 1499-1503 ◽  
Author(s):  
M D Ullman ◽  
R E Pyeritz ◽  
H W Moser ◽  
D A Wenger ◽  
E H Kolodny

Abstract Quantitative high-performance liquid chromatographic analysis of perbenzoylated sphingolipids has been used to study the correlations of body chemistry to clinical phenomena. Plasma sphingolipids were isolated from 32 Gaucher (β-glucosidase deficiency) and six Fabry (α-galactosidase deficiency) patients by solvent partition and chromatographic separation on silicic acid columns. Plasma sphingolipids from a patient undergoing plasma-exchange were separated from interfering lipids with reversed-phase columns. Liquid-chromatographic analysis of sphingolipids provides useful supportive information for diagnoses because affected individuals are shown to possess increased circulating concentrations of the pathognomonic sphingolipid. We also used this technique to monitor sphingolipid concentrations in plasma and urine sediment during plasma exchange of a p atient with Fabry’s disease. Regular plasma exchanges produced and maintained decreased concentrations of sphingolipids in plasma, but near pre-exchange concentrations were observed within days after the therapy was terminated.


1990 ◽  
Vol 73 (4) ◽  
pp. 595-598
Author(s):  
Stephen C Slahck

Abstract A liquid chromatographic method for determination of cyfluthrin (Baythrold®, Tempo®) diastereomers In technical and formulated products has been developed. Samples are dissolved in dloxane-hexane and analyzed by normal-phase liquid chromatography using acetophenone as an internal standard. The method Is applicable to technical Baythrold, Baythrold 2 EC, Tempo 20 WP, and granular formulations. The method separates all 4 diastereomers of cyfluthrin and all impurities in less than 19 mln.


2020 ◽  
Vol 12 (44) ◽  
pp. 5380-5391
Author(s):  
Yanawath Santaladchaiyakit ◽  
Supalax Srijaranai

A simple and rapid preconcentration method using dissolvable Mg/Al LDHs and SDS has been demonstrated for high performance liquid chromatographic analysis of benzoylurea insecticides in water and honey samples.


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