Abstract: A simple, rapid and versatile method for the separation and determination of sugars via high performance liquid chromatography is described. Virtually any combination of monosaccharides, disaccharides and/or higher oligomers can be separated. Detection via differential refractometry simplifies quantitative measurements and permits collection of emerging sugars for identifying tests. As little as 20 μg of an individual sugar can be determined and preliminary data indicate excellent precision and accuracy. Aqueous solutions of sugars, including samples containing substantial salts or other impurities, can be analyzed directly without derivatization or pretreatment.

Abstract: A simple automated analytical method for separation and quantitative determination of sugars from acidic and enzymatic hydrolysates of wood polysaccharides via borate complex ion exchange chromatography is described. Samples are analysed without any interferring manipulation like derivatization, deionization or deproteinization, and even sulphuric acid hydrolysates can be directly applied to the column. As little as 0.5 μg of an individual sugar can be quantitatively measured. Examples of the separation of common monomeric sugars and mixtures of mono-and disaccharides and uronic acids are given.

Abstract: Complex mixtures of O-trimethylsilylated polyamino alcohols, which have been generated by either acid or enzymatic hydrolysis of polypeptides and subsequent derivatization, are completely characterized by a gas chromatograph mass spectrometer computer system. These peptide derivatives possess excellent gas chromatographic properties; a wide range of derivatives from di- to hexapeptides may be separated in a single chromatographic experiment. The identification of these compounds, either manually or with the assistance of the computer, is based on three sets of data which are automatically generated after the g.c.m.s. computer experiment: (1) mass spectra, which exhibit sequence-determining ions of high abundance; (2) selected ion records, which allow efficient location of peptide derivatives in the gas chromatogram as well as resolution of incompletely separated fractions; (3) retention indices, which can be calculated from values which have been assigned to each amino acid residue.

Abstract: Bile and serum cholesterol concentrations were analyzed by the same saponification, extraction and gas chromatographic procedure, utilizing stigmasterol as an internal standard and trifluoroacetate derivatization. The method was rapid and highly sensitive, requiring only 20 to 50 mul of sample. Comparable levels of precision were achieved by parallel analysis of a series of bile and serum samples by the present method and the Abell colorimetric method; a high degree of correlation was found between these two methods.

Abstract: Advantages and disadvantages of derivatization-liquid chromatography are discussed. Distinction is made between pre-column and post-column techniques. Ion-pair chromatography is classified as a special form of pre-column technique. Some background aspects are mentioned briefly.

Abstract: Chromatographic methods, especially thin-layer chromatography (TLC) and gas-liquid chromatography (GLC) are widely used in investigations of the occurrence, molecular structure and metabolism of ether lipids. The application of such techniques to structural analysis and quantification, in combination with methods for the degradation and derivatization of ether lipids, is discussed.

Abstract: We present a method for separating and measuring guanidino acids by gas—liquid chromatography. Compared to ion-exchange techniques, this system is faster, more sensitive, requires smaller sample volumes, is independent of colorimetric reactions, and permits simultaneous determination of both amino and guanidino acids. N -Trifluoroacetyl- n -butyl esters are formed and then are separated by using a column containing a mixed silicone liquid phase coated on Chromosorb W-HP. Analytical recoveries from plasma ranged from 86 to 112% and were optimal when purification and derivatization were done without prior protein precipitation. Speculations as to the cause of this interference by protein include coprecipitation, protein-binding, and cyclization of the guanidines in the acids used for denaturation. Evidence presented suggests that all three occur: ultrafiltrability is diminished in the presence of protein and nuclear magnetic resonance demonstrates cyclization of some of these esters.

Abstract: Reconstructed mass chromatography using methane as a carrier and reagent gas for chemical ionization gas chromatography-mass spectrometry of the derived methyl esters allows rapid, quantitative microdeterminations of complete cholesteryl ester fatty acid profiles. The sensitivity of this method is consistent with completely specific, multicomponent assay at the picomole level. Introduction of two homologues as internal standards, one into the intact biological specimen and the other after derivatization, provides a measure of the net efficiency of the processes of extraction and derivatization. This procedure may be extended readily to the determination of fatty acid profiles in most biological fluids.

Abstract: In recent years the economic importance of herbicides has greatly exceeded that of other pesticides. Their use for weed control has had a tremendous impact on crop production as well as on management of non-agricultural land. They are being used in increased quantity and new compounds are being added to the list of herbicides every year. Thus, there exists an increasing demand for analytical methodology of herbicide residues.

Abstract: Publisher Summary This chapter discusses the gas-liquid chromatography (GLC) methods for chromatography of intact antibiotic molecules—mainly by derivatization. The chapter discusses some of the difficulties associated with quantitative derivatization and chromatography and describes precautionary measures for the successful GLC determination of antibiotics. Spectinomycin is chromatographed intact as the tetrakistrimethylsilyl derivative using an SE-52 column. Kanamyein is chromatographed intact as the silyl ether-silyl amine derivative using an OV-1 column. Neomycin is ehromatographed intact as the silyl ether-silyl amine derivative using an 0V-1 column. The procedure for the GLC analysis of paromomycin is analogous to that of neomycin powder. It follows the procedure as neomycin powder, using paromomycin in place of neomycin. Griseofulvin is chromatographed intact without derivatization using an OV-1 column. Cycloheximide is derivatized as the monotrimethylsilyl ether by treatment with isopropanol after silylation.

Abstract: L-Tryptophan is condensed with formaldehyde to yield 2,3,4,5-tetra-hydro-β-carboline-4-carboxylic acid. The trimethylsilyl derivative of this compound is suitable for selective ion monitoring during combined gas chromatography - mass spectrometry since it affords a relatively abundant molecular ion of high MSS.