McGregor R F, Sharon M S, Atkinson M, Johnson D E
Prep Biochem. 1976;6(6):403-19. doi: 10.1080/00327487608069126.
The isolation of polyamines from urinary hydrolysates in a sufficiently pure state for subsequent analysis by gas chromatography has proved to be difficult. However, by using columns of Porapak-Q and ion-exchange resins, urinary hydrolysates are readily purified and formation of trifluoroacetyl derivatives of polyamines proceeds in high yield without carryover of artifacts in the gas chromatographic elution profile. Good yields from the trifluoroacetylation reaction are not achieved if large quantities of salts or urinary pigments are present. By obtaining the polyamine carbonates in the final stages of the method described, the trifluoroacetylation reaction yields excellent derivatives of nanogram or microgram amounts, particularly after standing over-night at room temperature. The procedure described in detail should permit routine urinary polyamine analysis where rapidity, ease of handling many samples, freedom from complications and artifacts are a consideration.
从尿水解产物中分离出足够纯净的多胺,以便随后用气相色谱法进行分析,这已被证明是困难的。然而,通过使用Porapak-Q柱和离子交换树脂,尿水解产物很容易得到纯化,多胺三氟乙酰衍生物的形成产率很高,且在气相色谱洗脱图谱中不会携带假象。如果存在大量盐类或尿色素,则三氟乙酰化反应无法获得良好的产率。通过在所描述方法的最后阶段获得多胺碳酸盐,三氟乙酰化反应可产生纳克或微克量的优异衍生物,尤其是在室温下放置过夜后。详细描述的该程序应能实现常规尿多胺分析,此时需要考虑分析速度、易于处理多个样品、无并发症和假象等因素。