Capillary gas chromatographic determination of proteins and biological amino acids as N(O)-tert.-butyldimethylsilyl derivatives |
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| Institution: | 1. Global Cancer Institute, Boston, MA 02114, USA;2. Department of Hematology and Oncology, Instituto Nacional de Ciencias Médicas y Nutrición Salvador Zubirán, Mexico City, Mexico;3. Avon International Breast Cancer Program, Massachusetts General Hospital Cancer Center, Boston, MA 02114, USA;4. Cancer Care in the Elderly Clinic, Department of Geriatrics, Instituto Nacional de Ciencias Médicas y Nutrición Salvador Zubirán, Mexico City, Mexico;5. Department of Clinical Oncology, Hospital de Clínicas de Porto Alegre, Porto Alegre, RS, Brazil;6. Mae de Deus Cancer Institute, Hospital Mae de Deus, Porto Alegre, RS, Brazil;7. Biostatistics Center, Massachusetts General Hospital, Boston, MA 02114, USA;8. Massachusetts General Hospital Cancer Center, Boston, MA 02114, USA;9. Mater Misericordiae University Hospital, Dublin, Ireland;1. Impacts and Astromaterials Research Centre, Department of Earth Science and Engineering, South Kensington Campus, Imperial College London, SW7 2AZ, UK;2. Space Research Centre, Michael Atiyah Building, Department of Physics and Astronomy, University of Leicester, Leicester LE1 7RH, UK;3. Cranfield Health, Vincent Building, Cranfield University, Bedfordshire MK43 0AL, UK;1. Max Planck Institute for Solar System Research, Göttingen, Germany;2. LISA—Laboratoire Interuniversitaire des Systèmes Atmosphériques, CNRS/Universités Paris Est Créteil & Paris Diderot, Créteil, Paris, France;3. University of Bremen, Institute for Applied and Physical Chemistry, Bremen, Germany;4. Université Versailles St-Quentin, Sorbonne Universités, UPMC Univ. Paris 06, CNRS/INSU, LATMOS-IPSL, 78280 Guyancourt, France;5. Leiden Observatory, P.O. Box 9513, 2300 RA Leiden, The Netherlands;6. Space Policy Institute, George Washington University, 20052 Washington, DC, USA;7. University of Houston-Clear Lake, Houston, TX, USA;8. Space Technology Ireland, Ltd., National University of Ireland, Maynooth, Co., Kildare, Ireland;9. Université Nice Sophia Antipolis, Institut de Chimie de Nice, UMR 7272 CNRS, Nice, France;10. Centro de Astrobiología, INTA-CSIC, E-28850 Torrejón de Ardoz, Madrid, Spain;11. German Aerospace Center, DLR, Cologne, Germany;1. Department of Plant Pathology, Physiology, and Weed Science, Virginia Tech, Blacksburg, VA 24061-0390, USA;2. Department of Civil and Environmental Engineering, Virginia Tech, Blacksburg, VA 24061-0246, USA;1. Aix-Marseille Université, PIIM UMR-CNRS 7345, F-13397 Marseille, France;2. Univ. Paris-Sud, Université de Paris-Saclay, Astrochimie et Origines, Institut d’Astrophysique Spatiale, UMR 8617, Orsay 91405, France;3. Université Grenoble Alpes, CNRS, IPAG, Grenoble F-38000, France;4. CNRS, Orsay 91405, France |
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| Abstract: | Forty-seven biological amino acids containing all 22 protein amino acids were derivatized to N(O)-tert.-Butyldimethylsilyl (tBDMSi) derivatives by a single-step reaction with N-methyl-N-(tert.-butyldimethylsilyl)trifluoroacetamide and successfully separated on an HP-1 capillary column. The relative standard deviations of the relative molar responses of most amino acids were <5%. Cystine seems to be partially converted into cysteine during derivatization. An increase in carrier gas flow-rate towards the end of the analysis by inlet pressure programming with electron pressure control avoided the peak broadening and adsorption of the derivatives with high boiling points on the column and especially increased sensitivity of cystine to 5 pmol. Glutamine was converted almost completely into pyroglutamic acid during prolonged storage of a standard solution prepared in 0.01 M HCl but not during derivatization. These results compared with those for the phenylthiocarbamyl derivatives analysed by HPLC and the analytical results reported in the literature on soybean hydrolysate showed good agreement except for cysteine. The results for the amino acid composition of bovine serum albumin also showed good agreement with results in the literature except for cysteine. In human urine, seventeen free amino acids were detected as tBDMSi derivatives. |
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