Liquid Chromatographic Apparatus for Quantitative Analysis

1966 ◽  
Vol 44 (23) ◽  
pp. 2805-2811 ◽  
Author(s):  
S. Kašpárek ◽  
R. A. Heacock

In contrast to previous reports in the literature, it has been shown that both 1- and 3-carbethoxyindole are obtained from the reaction of indole magnesium iodide with 1 or 2 moles of ethyl chloroformate. The formation of 1-carbethoxyindole was favored at low temperatures (i.e. −10°), whereas maximum yields of 3-carbethoxyindole were obtained at 10°. Significant quantities of 1,3-dicarbethoxyindole are only formed in the presence of 2 equivalents of ethyl chloroformate and when the reaction is carried out at higher temperatures (i.e. 35°).Paper and gas–liquid chromatographic systems have been developed for the qualitative and quantitative analysis of mixtures containing indole, 1-, 2-, and 3-carbethoxyindole, and 1,3-dicarbethoxyindole.


1976 ◽  
Vol 59 (1) ◽  
pp. 162-164
Author(s):  
Samuel K Reeder

Abstract A method is presented for the quantitative analysis of o-phenylphenol residues in citrus oils, encapsulated flavors, and dried meal. The method utilizes high-speed liquid chromatography for the determination after specific sample preparations for each material. These preparations include hexane extraction of acidified basic extracts or steam distillation and extraction. The limit of the analysis is <1 ppm with an analysis time of <45 min.


1988 ◽  
Vol 71 (4) ◽  
pp. 707-709
Author(s):  
Jim L Weigand ◽  
Daniel S Dille

Abstract Melengestrol acetate (MGA) is determined by liquid chromatography using a fraction from preparatory LC as a means of sample cleanup for feedstuffs, both dry and liquid. Dry ground feed is Soxhlet extracted with hexane and passed through a 2% deactivated alumina column for initial cleanup. The eluate is evaporated, redissolved in methanol, filtered, and injected onto a preparatory LC column. The fraction containing MGA is separated from the remaining matrix, evaporated to dryness, dissolved in methanol, and quantitated by LC analysis. Liquid supplements are extracted in methanol, and the extract is evaporated to near dryness. The residue is diluted with water, extracted with chloroform, passed through sodium sulfate, and evaporated to dryness. The remaining sample is dissolved in methanol prior to preparative LC and quantitative LC. Recoveries for 2 laboratory- fortified commercial feeds, one dry and one liquid, containing 0.39 and 0.40 mg/lb, were 98.3% ± 4.4 and 95.8% ± 4.3, respectively. Results compare favorably with existing methods. Up to a 4-fold time savings was realized by this method without automation.


1985 ◽  
Vol 74 (6) ◽  
pp. 664-667 ◽  
Author(s):  
Robert C. Gaver ◽  
Hassan S. Movahhed ◽  
Raymond H. Farmen ◽  
Kenneth A. Pittman

1982 ◽  
Vol 207 (3) ◽  
pp. 599-603 ◽  
Author(s):  
Anthony H. Jackson ◽  
K. R. Nagaraja Rao ◽  
Sydney G. Smith

New high-pressure-liquid-chromatographic methods have been developed for the quantitative analysis of mixtures of coproporphyrins I and III, and of isocoproporphyrin, dehydroisocoproporphyrin and de-ethylisocoproporphyrin.


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