Effective Hydrolysis and Clean-up Methods for the Analysis of Amino Acid Composition in Food Proteins using N(O)-tert.-butyldimethylsilyl Derivative by GC

Woo, Kang-Lyung;Jang, Duck-Kyu;Kim, Je-I;Woo, Dong-Kyun;Lee, Yu-Weon

  • Published : 20020600

Abstract

To improve the accuracy of amino acid analysis on food samples, several hydrolysis methods and clean-up procedures on the protein hydrolysate were investigated. The hydrolysis by 6 M HCOOH containing 0.3% tryptamine was an excellent method for the standard protein, bovine serum albumin, showing results which were very closed to theoretical values on the standard amino acids and sequencing values reported in the literatures. The recoveries determined from the clean-up methods using the classical cation-exchange and $C_{18}$ Sep-Pak cartridge on the standard amino acids were similar. However, $C_{18}$ cartridge could not be used in the food sample because it did not remove the high molecular weight and hydrophobic compounds. The N(O)-tert.-butyldimethylsilyl derivatives of 22 amino acids were completely resolved on the Ultral capillary column by GC and GC/MSD. EI mass spectra of tBDMSi amino acid esters were characterized with M-15, M-57, M-85, M-159, M-R, m/z $147 [(CH_3)_3 SiO= Si(CH_3)_2]$, $133 [(CH_3)_2HSiO^+=Si(CH_3)_2]$ and $73 [(CH_3)_3Si]$.

Keywords

References

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