Chemical Methods in Gas Chromatography by V. G. Berezkin

By V. G. Berezkin

During this two-part monograph, the writer describes smooth equipment for the fast column liquid chromatography of excessive- and medium-molecular-weight compounds of organic foundation, i.e. proteins, peptides, enzymes, nucleic acids, poly- and oligonucleotides, poly- and oligosaccharides, advanced biopolymers and biooligomers comparable to viruses, bacteriophages, ribosomes and glycoconjugates, in addition to another compounds corresponding to immunomodulators. the fabric is contained in elements: half A facing basic chromatographic conception, rules, fabrics and methods; and half B facing the separation of person compound sessions and containing a check in of chromatographed components and a full-title bibliography. not just is that this a really expert, exact treatise on chromatographic concepts, it additionally provides a vast, balanced overview of speedy separation of all identified very important biopolymers and biooligomers, either basic and intricate, and likewise of a few synthetically ready and pharmaceutically vital biooligomers. moreover, it presents an creation to the applying of HPLC to the examine of the constitution of those components.

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The analysis of barbiturates is an important practical task. 2 STRUCTURAL FORMULAE OF BARBITURATES [39] Compound R, R* R3 1 Methabarbital 2 3 Barbital Allobarbital Ethyl Ethyl Allyl Methyl Hydrogen Hydrogen Hydrogen No. 4 Aprobarbital Allyl Ethyl Ethyl Allyl Isopropyl 5 5,5-Dipropylbarbituric acid Propyl Propyl Hydrogen Butethal Amobarbital Pentobarbital Vinbarbital Secobarbital Ethyl Ethyl Ethyl Ethyl Allyl Butyl 3-Methylbutyl 1-Methylbutyl l-Methylbutenyl l-Methylbutyl Hydrogen Hydrogen Hydrogen Hydrogen Hydrogen Hexobarbital Methyl l-Cyclohexenyl Methyl Ethyl Allyl Phenyl Phenyl Hydrogen Hydrogen Ethyl l-Cy clopentenyl Hydrogen 6 I 8 9 10 11 12 13 14 15 Glut e thimide Phenobarbital 5-Allyl-5-phenylbarbituricacid Hep tobarb Ehrsson [40]) and subsequent GC analysis on a glass surface-layer capillary column.

1 = Desoxypyridoxine; 2 = pyridoxine; 3 = unidentified; 4 = pyridoxal; 5 = pyridoxamine. From ref. 95. , the mass spectrometer [89]. The use of a mass spectrometer as the detector enables one to record chromatograms at two or three different fixed mass spectral lines (the ‘mass fragmentation’ or ‘selected ion detection’ method [90-93]), which makes it possible, when the lines in mass spectra have been chosen correctly for recording, to determine selectively even those compounds that form a common chromatographic peak.

To form the derivatives of trifluoroacetic acid 3 0 ~ of 1 N-methylbistrifluoroacetamide were added [97], the lid was closed and the vial was heated for 20 min. After cooling, the sample was placed directly in the chromatograph for quantitative analysis. ) packed with 5% silicone DC-550 on Chromosorb P AW DMCS. The chromatogram is shown in Fig. 16. The limit of determination for an FID is about 250ng. Meesschaert et al. [98] proposed a technique for analysing natural penicillins in the form of their methyl ethers.

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