Gas-liquid chromatography of protein amino acid trimethylsilyl derivatives

Gehrke, Charles W.; Nakamoto, Hiromasa; Zumwalt, Robert W.

doi:10.1016/s0021-9673(01)86179-3

Cited by 124 publications

(29 citation statements)

References 13 publications

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“…Usually, a silylation is carried out. Formerly, BSTFA [1] was the silylation method of choice; however, anhydrous conditions and continuous heating were required. Moreover, the silylation conditions reported by Gehrke and coworkers were sometimes contradictory.…”

Section: Introductionmentioning

confidence: 99%

Comparison of silylation and esterification/acylation procedures in GC‐MS analysis of amino acids

Sobolevsky¹,

Revelsky

Miller

et al. 2003

J of Separation Science

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Three derivatization agents used in GC analysis of amino acids were compared: N,O‐bis(trimethylsilyl)trifluoroacetamide, (BSTFA), N‐methyl‐N‐(tert‐butyldimethylsilyl)trifluoroacetamide (MTBSTFA), and isobutyl chloroformate (iBuCF). It was shown that the analytical characteristics achieved in the case of silylation with MTBSTFA are comparable to those obtained for esterification/acylation. However, since the former approach requires laborious sample preparation to isolate the compounds in question prior to derivatization, determination of amino acids as N(O,S)‐alkoxycarbonyl alkyl esters seems to be preferable in many cases. Application of the esterification/acylation procedure to analysis of lyophilized E. coli microbial culture was demonstrated.

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Section: Introductionmentioning

confidence: 99%

Comparison of silylation and esterification/acylation procedures in GC‐MS analysis of amino acids

Sobolevsky¹,

Revelsky

Miller

et al. 2003

J of Separation Science

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“…SH, OH, NH and COOH) with nonpolar trimethylsilane groups (TMS). According to some studies, by replacing acidic protons with nonpolar TMS groups, polarity of an amino acid is reduced and its vola" lity is increased [11][12][13][14][15][16][17] which is an advantage in gas chromatographic analysis.…”

Section: Resultsmentioning

confidence: 99%

Method for determination of amino acid content in protein products for medical use

Macovescu¹,

Chelaru²,

Gurau³

2017

LFJ

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ABSTRACT. The paper presents a method for determina$ on of amino acid content in collagen biomaterials for medical use produced in the Collagen Department of INCDTP -Division ICPI and its valida$ on. The method has three stages: the fi rst consists in hydrolysing the collagen biomaterial sample down to amino acids; the second step refers to deriva$ za$ on of amino acids with N, O-bis (trimethylsilyl) trifl uoroacetamide (BSTFA) which is a silyla$ on reagent; deriva$ zed amino acids are detected using a mass spectrometer a+ er gas chromatography. The method was validated to establish performance parameters and to check compliance with the intended purpose. KEY WORDS: collagen, amino acids, biomaterials METODĂ PENTRU DETERMINAREA CONŢINUTULUI DE AMINOACIZI DIN PRODUSELE PROTEICE PENTRU UZ MEDICALREZUMAT. Se prezintă o metodă de determinare a conţinutului de aminoacizi din biomaterialele colagenice pentru uz medical produse în Departamentul Colagen al INCDTP -Sucursala ICPI şi validarea ei. Metoda are trei etape: prima constă în hidroliza probei de biomaterial colagenic până la stadiul de aminoacizi; a doua etapă se referă la deriva$ zarea aminoacizilor cu N, O-bis (trime$ lsilil) trifl uoracetamidă (BSTFA) care este un reac$ v de sililare; aminoacizii deriva$ zaţi sunt detectaţi pe un spectrometru de masă după gaz cromatografi e. Metoda a fost validată pentru a se stabili parametrii de performanţă şi pentru verifi carea conformării cu scopul propus. CUVINTE CHEIE: colagen, aminoacizi, biomateriale PROCÉDÉ DE DÉTERMINATION DE LA TENEUR EN ACIDES AMINÉS DANS DES PRODUITS PROTÉIQUES À USAGE MÉDICALRÉSUMÉ. On présente une méthode de détermina$ on de la teneur en acides aminés de biomatériaux de collagène à usage médical fabriqués dans le Département Collagène de INCDTP-ICPI et sa valida$ on. La méthode comporte trois étapes : la première consiste en l'hydrolyse de l'échan$ llon de biomatériau de collagène au stade des acides aminés ; la deuxième étape se rapporte à la dériva$ sa$ on d'acides aminés avec du N, O-bis (triméthylsilyl) trifl uoroacétamide (BSTFA) qui est un réac$ f de silyla$ on ; les acides aminés dérivés sont détectés sur un spectromètre de masse après chromatographie en phase gazeuse. La méthode a été validée pour établir les paramètres de performance et vérifi er la conformité avec l'objec$ f prévu.

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“…Two systems were employed: that of Coulter and Hann (1968), in which the n-propyl-Nacetyl esters of the amino acids are formed, and that of Gehrke, Nakamoto, and Zumwalt (1969), in which the N-trimethylsilyl esters are prepared using bis(trimethylsilyl)trifluoroacetamide (BSTFA). Some modifications which favoured the separation of certain selenoamino acids were made from the method of Gehrke, Nakamoto, and Zumwalt (1969).…”

Section: (Iv) Gas-liquid Ohromatography (Glo)mentioning

confidence: 99%

“…Some modifications which favoured the separation of certain selenoamino acids were made from the method of Gehrke, Nakamoto, and Zumwalt (1969).…”

Section: (Iv) Gas-liquid Ohromatography (Glo)mentioning

confidence: 99%

Identification of [75se]Selenomethionine in Ewe Milk Protein Following the Intraruminal Administration of Na75seo3 as a Single Oral Dose

Godwin¹,

Handreck²,

Fuss³

1971

Aust. Jnl. Of Bio. Sci.

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Inorganic selenium, as Na275Se03, was given intraruminally to lactating ewes, and for 48 hr afterwards samples of blood and milk were taken regularly. The animals were then slaughtered and tissues taken for further analysis. Evidence is presented, based on isolation techniques using Sephadex chromatography and gas-liquid chromatography, that 75Se is incorporated into milk proteins as selenomethionine_ It is estimated that at least 3% of the selenium that enters the milk, from this inorganic source, is present as bound selenomethionine. This is a minimal value, since it has been shown that selenomethionine is easily degraded during a number of the isolation procedures.The steps followed in arriving at the conclusion were: (1) a large proportion of the 75Se activity in the milk was non-dialysable; (2) activity emerges with the milk protein on Sephadex and can be recovered as "soluble casein" by precipitation with ammonium sulphate; (3) Pronase digestion of the labelled protein produces fragments that behave like methionine and cysteine in column chromatography; and (4) gas-liquid chromatography, including collection of the effluent in fractions, has enabled positive identification of a [75SeJselenomethionine peak_Other selenoamino acid-like fractions are present but have not yet been identified.

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Gas-liquid chromatography of protein amino acid trimethylsilyl derivatives

Cited by 124 publications

References 13 publications

Comparison of silylation and esterification/acylation procedures in GC‐MS analysis of amino acids

Comparison of silylation and esterification/acylation procedures in GC‐MS analysis of amino acids

Method for determination of amino acid content in protein products for medical use

Identification of [75se]Selenomethionine in Ewe Milk Protein Following the Intraruminal Administration of Na75seo3 as a Single Oral Dose

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