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• W2017302807 abstract "The GC analysis of amino acids such as the N-trifluoroacetyl (N-TFA) n-butyl esters – the established method developed principally in our laboratories – provides an effective and reliable means of amino acid determination that is applicable to a very wide range of analytical needs. My research group, graduate students, and colleagues during the period from 1960 to 1975, established the fundamentals of quantitative derivatization, conditions of chromatographic separation, and defined the interactions of the amino acid derivatives with the stationary and support phases. Our studies and continued refinements since 1974 have resulted in a precise and accurate, reliable, straightforward method for amino acid measurement [[1], [2], [3], [4]].We conducted an extensive array of the applications of GC of amino acid analysis on a wide range of sample matrices, from pine needle extracts to erythrocytes. The Experimental section developed (Volume 1, Chapter 1) [2] provides a thorough description of our quantitative analytical procedures, including preparation of ethylene glycol adipate (EGA) and silicone-mixed phase chromatographic columns. The EGA column which is used to separate and quantitate all the protein amino acids, except histidine, arginine, and cystine is composed of 0.65 w/w% stabilized grade EGA on 80/100 mesh acid-washed Chromosorb ® W, 1.5 m × 4 mm ID glass. For quantitation of histidine, arginine, and cystine, the silicone-mixed phase of 1.0 w/w% OV-7 and 0.75 w/w% SP-2401 on 100/120 mesh Gas-Chrom® Q (1.5 m × 4 mm I.D. glass) performs extremely well. We also describe the preparation and use of ion-exchange resins for sample cleanup, and complete sample derivatization to the N-TFA ≪-butyl esters. The amino acids are esterified by reaction with rc-butanol • 3 N HC1 for 15 min at 100°C and the excess ≪-butanol’ 3 N HC1 is removed under vacuum at 60°C any remaining moisture is removed azeotropically with dichloromethane; then the amino acid esters are trifluoroacylated by reaction with trifluoroacetic anhydride (TFAA) at 150° C – 5 min in the presence of dichloromethane as solvent. Immediately following the Experimental section are valuable comments on various parts of the method [3], which provide guidance to the use of the entire technique, from sample preparation to chromatography to quantitation. Of particular value is a comparison of GLC and IEC results of hydrolysates of diverse matrices. This extensive comparison of an array of sample types showed that the values obtained by the two techniques were generally in close agreement.The analysis of amino acids as the N-'IFA ≫-butyl esters is an established technique that offers much to scientists concerned with the determination of amino acids. The method offers excellent precision, accuracy, selectivity, and is an economical complementary technique to the elegant Stein-Moore ion-exchange method.We also provide both a detailed account and historical perspective on development of GC amino acid analysis and describe the solution of problems encountered as the methods evolved [2]. The N-TFA w-butyl ester and trimethylsilyl (TMS) derivatives are discussed, including reaction conditions, chromatographic separations, mass spectrometric (MS) identification of both classes of derivatives, interactions of the arginine, histidine, and cystine derivatives with the liquid phase and support materials, and application of the methods in (Volume 1, Chapter 3) [2]. The acylation of arginine posed a problem in early studies; the successful solution of this problem paved the way to a high-temperature acylation procedure, which is now widely used with numerous acylating reagents [[5], [6], [3]] Likewise, esterification of the amino acids was investigated in detail, resulting in a direct esterification procedure which quickly and reproducibly converts the amino acids to ≪-butyl esters. This approach has also been widely used to form various amino acid esters [3].The early development of GLC analysis of iodine- and sulfur-containing amino acids as the TMS derivatives is described, with the finding that bis (trimethylsilyl)trifluoroacetamide (BSTFA), a silylating reagent which we invented and patented, is an effective silylating reagent to form amino acid derivatives (Volume 1, Chapter 3) [[2], [6]]. Our studies on the derivatization of the protein amino acids with our silylation reagent, BSTFA, led the conversion of the amino acids to volatile derivatives in a single reaction step. Although certain amino acids tend to form multiple derivatives which contain varying numbers of TMS groups, high-temperature, long reaction time derivatization permits quantitative analysis of the amino acids as the TMS derivatives. Our studies on the GLC of the TMS amino acids resulted in the development of a 6 m column of 10% OV-11 on Supelcoport® for separation of the TMS derivatives.The development of a chromatographic column system for the VV-TFA ≪-butyl esters came about from the realization that the derivatives of arginine, histidine, and cystine were not reproducibly eluted from columns with polyester liquid phases, although this type of column was excellent for analysis of the other protein amino acids. We developed a siloxane mixed phase column specifically for these three amino acids, with the final system being an ethylene glycol adipate (EGA) column for 17 amino acids and the mixed phase column for the remaining 3 [[5], [6]]. Our summary points out, that the foundation of a successful amino acid analysis by GC is composed of two elements: (a) reproducible and quantitative conversion of amino acids to suitable derivatives, and (b) separation and quantitative elution of the derivatives by the chromatographic column.A literature review is presented for the period of 1984 to 2005 on topics ranging from N-acyl O-esters of amino acid derivatives to: Enantiomeric composition, racemization, gas chromatographic enantiomer separation, formation of volatile derivatives, mass spectrometric analysis of cyclosporine metabolites, GC of 1- and 3-methyl histidine in biological fluids, rapid analyses, resolution of sulfur-containing amino acids on chiral columns, simultaneous derivatization of functional groups with one-step ethyl chloroformate derivatization, derivatization of chiral amino acids in supercritical CO2, separation of diasteromeric esters of a-alkyl- a-amino acids, and capillary GC plus numerous other subjects on GC of amino acids (see titles and authors as follows)." @default.
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• W2017302807 date "1967-01-01" @default.
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• W2017302807 title "The preparation of diazopropane and diazobutane for the esterification of amino acids" @default.
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• W2017302807 doi "https://doi.org/10.1016/s0021-9673(01)98906-x" @default.
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