Rotgans J, Wodarz R, Schoknecht W, Drysch K
Arch Oral Biol. 1983;28(12):1121-4. doi: 10.1016/0003-9969(83)90168-1.
The use of polysiloxanes as stationary phase in glass-capillary gas-chromatography carrying chiral groups enables the separation and quantitation of most amino-acid enantiomers and a variety of other compounds in a much shorter time than previously. This phase exhibits low volatility and high thermal stability and may be used in routine analysis with open tubular columns at temperatures of at least 175 degrees C. Most protein amino acids are separated in a temperature programme between 90 and 175 degrees C, thus obviating the need for multiple injections. Resolution factors are lower than those of other diamide phases containing the L-valine-t. butyl-amide group, but are sufficient for resolution of almost all protein amino-acid enantiomers. Incomplete recovery from the sample, incomplete derivatization, hydrolysis and thermal decomposition of the derivative and shifting response factors can be compensated for by adding the unnatural enantiomer. The accuracy of amino-acid analysis by enantiomer labelling is equal or superior to that of known methods and permits complete analysis of peptides with respect to both amino-acid composition and the optical purity of each amino acid. The application of this method to human saliva provided information concerning enzymic and bacterial process in the mouth.
在带有手性基团的玻璃毛细管气相色谱中使用聚硅氧烷作为固定相，能够在比以前短得多的时间内分离和定量大多数氨基酸对映体以及多种其他化合物。该固定相具有低挥发性和高热稳定性，可用于内径开口柱的常规分析，温度至少为175摄氏度。大多数蛋白质氨基酸在90至175摄氏度的程序升温中被分离，从而无需多次进样。分离因子低于其他含有L-缬氨酸叔丁酰胺基团的二酰胺固定相，但足以分离几乎所有蛋白质氨基酸对映体。通过添加非天然对映体，可以补偿样品回收不完全、衍生化不完全、衍生物的水解和热分解以及响应因子的变化。通过对映体标记进行氨基酸分析的准确度与已知方法相当或更高，并且能够就氨基酸组成和每种氨基酸的光学纯度对肽进行完整分析。将该方法应用于人类唾液，提供了有关口腔中酶促和细菌过程的信息。
