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Selective determination of secondary amines as their N ‐diethylthiophosphoryl derivatives by gas chromatography with flame photometric detection
Author(s) -
Kataoka Hiroyuki,
Eda Michiko,
Makita Masami
Publication year - 1993
Publication title -
biomedical chromatography
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.4
H-Index - 65
eISSN - 1099-0801
pISSN - 0269-3879
DOI - 10.1002/bmc.1130070304
Subject(s) - chemistry , chromatography , amine gas treating , gas chromatography , calibration curve , urine , primary (astronomy) , detection limit , gas chromatography–mass spectrometry , mass spectrometry , organic chemistry , biochemistry , physics , astronomy
A selective and sensitive method has been developed for the determination of secondary amines by gas chromatography (GC). After removal of primary amines by the reaction with o ‐phthaldialdehyde, secondary amines were converted into their N ‐diethylthiophosphoryl derivatives and then measured by GC with flame photometric detection using a DB‐1701 capillary column. The derivatives were sufficiently volatile and stable to give single symmetrical peaks. The detection limits of secondary amines were ca. 0.05‐0.2 pmol per injection. N ‐Methylcyclohexylamine was used as an internal standard. The calibration curves for secondary amines in the range 1–20 nmol were linear and sufficiently reproducible for quantitative determination. This method was successfully applied to small urine samples without prior clean‐up. Overall recoveries of secondary amines added to urine samples were 91–105%. By using this method, secondary amines in urine samples could be analysed without any influence from primary amines and other coexisting substances. The analytical results of secondary amine content in urine samples of normal subjects are presented.