Early R J, Thompson J R, McAllister T, Fenton T W, Christopherson R J
J Chromatogr. 1984 Sep 14;310(1):1-10. doi: 10.1016/0378-4347(84)80062-6.
A method is given for the quantitative analysis of the alpha-keto derivatives of the branched-chain amino acids in physiological fluids. A sample containing alpha-ketovalerate and alpha-ketocaproate as internal standards is passed through a weak anion-exchange resin at neutral pH. After washing the resin with distilled water, the alpha-keto acids are eluted with 4 M hydrochloric acid--ethanol (50:50). Quinoxalinol derivatives are prepared directly in the eluent, extracted with methylene chloride, and trimethylsilylated. Separation of the derivatives is by capillary gas chromatography on a 30 m fused-silica SE-30 column. Chromatographic separation is superior to that reported for packed column methods, thereby permitting the use of alpha-ketovalerate and alpha-ketocaproate as internal standards.
给出了一种定量分析生理体液中支链氨基酸α-酮衍生物的方法。将含有α-酮戊酸酯和α-酮己酸酯作为内标的样品在中性pH条件下通过弱阴离子交换树脂。用蒸馏水洗涤树脂后，用4M盐酸-乙醇（50:50）洗脱α-酮酸。直接在洗脱液中制备喹喔啉醇衍生物，用二氯甲烷萃取并进行三甲基硅烷化。衍生物通过在30m熔融石英SE-30柱上进行毛细管气相色谱分离。色谱分离优于报道的填充柱方法，从而允许使用α-酮戊酸酯和α-酮己酸酯作为内标。
