By V. G. Berezkin
During this two-part monograph, the writer describes smooth equipment for the quick column liquid chromatography of excessive- and medium-molecular-weight compounds of organic beginning, i.e. proteins, peptides, enzymes, nucleic acids, poly- and oligonucleotides, poly- and oligosaccharides, advanced biopolymers and biooligomers akin to viruses, bacteriophages, ribosomes and glycoconjugates, in addition to another compounds corresponding to immunomodulators. the cloth is contained in elements: half A facing basic chromatographic concept, ideas, fabrics and methods; and half B facing the separation of person compound sessions and containing a sign up of chromatographed ingredients and a full-title bibliography. not just is that this a really expert, exact treatise on chromatographic thoughts, it additionally offers a wide, balanced evaluate of speedy separation of all identified very important biopolymers and biooligomers, either uncomplicated and intricate, and likewise of a few synthetically ready and pharmaceutically very important biooligomers. furthermore, it presents an creation to the appliance of HPLC to the learn of the constitution of those elements.
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Additional resources for Chemical Methods in Gas Chromatography
By saponification, aminolysis or alcoholysis) and their GC analysis. As an example let us consider the work of Allen et al. [ 3 7 ] , devoted to elaborating a quantitative method for determining the monomers (repetitive structural units) in polyesters, the first stage of which was alkaline hydrolysis by a solution of potassium hydroxide in 2-ethoxyethanol. After hydrolysis the mixture was acidified by adding ~~ Fig. 1. Chromatograms of 50 amino acids in the form of their isobutylestersof N-heptafluorobutyric derivatives (331.
Chromatograms o f trimethylsilyl glycols. Reprinted with permission from ref. 37. Fig. 3. Chromatograms of trimethylsilyl ethers of high-boiling acids. Reprinted with permission from ref. 37. concentrated hydrochloric acid, and pyridine was added to dissolve the acids. A 50-pl volume of the reaction mixture was then added to 5OOpl of N,O-bis(trimethylsily1)trifluoroacetamide (BSTFA) to obtain ethers and esters of the alcohols and acids formed. 1 -pl sample. Fig. These products were obtained by analysing an experimental sample of polyether.
The dependence of the yield of the ester on the time of alkylation is shown in Fig. I 1. It follows from the data presented that in the best instance the time necessary for a 100% yield is 30min. The authors showed, however, that the duration of reaction can be reduced if the reaction is made coincident with the evaporation stage, when the reaction rate increases radically, apparently as a resuIt of an increase in temperature and the concentration of reagents. Investigation of the completeness of reaction is a necessary stage in the elaboration of a quantitative method, with slight changes in the structure of sample compounds being capable of radically affecting the rate of derivative formation.
Chemical Methods in Gas Chromatography by V. G. Berezkin