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KMID : 0366919970090010036
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Sungkyun Pharmceutical Journal
1997 Volume.9 No. 1 p.36 ~ p.45
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Rapid gas chromatographic profiling and screening of biologically active amines
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Kim, Kyoung Rae
Paik, Man Jeong/Kim, Jung Han/Dong, Suk Won/Jeong, Do Hyeon
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Abstract
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An efficient method is described for the simultaneous determination of 57 amines including volatile aliphatic amines, nonvolatile polyamines and catecholamines present in aqueous samples. The mothod is based on two-phase isobutyloxycarbonylation (isoBOC) with a pH shift. In 1.0 M phosphate buffer at pH 7.5, phenolic hydroxyl groups were allowed to react with isobutyl chloroformate in the dichloromethane phase, and subsequently pH of the aqueous phase was increased to 12.0 for the reaction of basic amino functions. The resulting N(O)-isoBOC amines were recovered by solid-phase extraction using Chromosorb P in normal phase partition mode, with subsequent tert.-butyldimethylsilylation of the remaining hydroxyl groups for gas chromatographic analysis. Using this combined procedure, linear responses were obtained in the concentration range of 0.2-12 ppm, with correlation coefficients varying from 0.945 to 0.999 for most of the amines studied except for 5-methoxytryptamine (0.864). Temperature-programmed retention index(I) sets as measured on DB-5 and DB-17 dual-capillary columns of different polarity were characteristic of each amine and thus, useful in the screening for amines by computer I matching. When applied to saliva samples, the present method allowed rapid screening for each spiked amine and unspiked polyamines such as 1,3-diaminopropane, putrescine, cadaverine and spermidine.
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