University of North Florida
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Stuart Chalk, Ph.D.
Department of Chemistry
University of North Florida
Phone: 1-904-620-1938
Fax: 1-904-620-3535
Email: schalk@unf.edu
Website: @unf

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Amines, secondary

@ ChemSpider@ NIST@ PubChem

Citations 3

"Flow Injection Determination Of Secondary Amines In Nonaqueous Solution With Fluorescence Detection"
Anal. Chim. Acta 1988 Volume 204, Issue 1-2 Pages 343-348
I. R. C. Whiteside and P. J. Worsfold, E. H. McKerrell

Abstract: A non-aqueous flow injection method is described for the selective determination of secondary amines, based on derivatization with 7-chloro-4-nitrobenzofurazan(I) to form fluorescent adducts. Primary amines are chemically masked online with an equimolar mixture (58 mM) of phthalaldehyde(II) and 2-mercaptoethanol(III) in ethyl acetate. Both reagents are pumped at 0.5 mL min-1. Samples (20 µL) are injected into the II - III stream and merged with the I stream for reaction at 45°C. Fluorimetric detection is at 525 nm (excitation at 480 nm). The detection limits for dibutyl-, dihexyl- and didecyl-amine were 0.08, 0.06 and 0.12 mM, respectively. The coefficient of variation for 0.34 mM dihexylamine was 1.3% (n = 5).
Fluorescence Heated reaction

"Fluorimetric Determination Of Secondary Amines By High Performance Liquid Chromatography With Post-column Derivatization"
J. Chromatogr. A 1983 Volume 264, Issue 3 Pages 423-433
Akira Himuro, Hiroshi Nakamura and Zenzo Tamura

Abstract: Amines were separated on columns (25 cm x 4.6 mm or 30 cm x 4.0 mm) of, respectively, Partisil-10 SCX or TSK LS-410; the respective mobile phase (pH 3) was 0.1 M citrate or ~50 mM phosphate buffer. The eluate was mixed with NaClO solution to convert secondary into primary amines; the reaction also decreased the detectability of primary amines with phthalaldehyde - 2-mercaptoethanol reagent. The products of reaction with the cited reagent (after addition of 2,2'-thiodiethanol to reduce excess of NaClO) were determined by fluorimetry at >405 nm (excitation at 360 nm). The optimum pH value and NaClO concentration. were: for prolines, ~8 and 0.03 mM, ~12 and 0.07 mM for adrenaline and 3-O-methyladrenaline, and ~14 and 0.15 mM for N-methylamino-acids (e.g., sarcosine). In an example, catecholamines and their 3-O-methyl derivatives were efficiently separated on the TSK column in ~40 min. Typically, the coefficient of variation for 1 nmol injected (n = 10) was 2.7% for proline and 1.7% for 4-aminobutyric acid.
HPLC Fluorescence Post-column derivatization

"Selective Fluorogenic Flow Injection Procedures For Primary, Secondary, And Tertiary Amines In Nonaqueous Media"
Anal. Proc. 1988 Volume 25, Issue 3 Pages 60-61
I. R. C. Whiteside, P. J. Worsfold, A. Lynes, E. H. McKerrell

Abstract: Three different reagent systems were used with an apparatus that included a 1-m reaction coil operated at 45°C and an LS-2 fluorimetric detector (Perkin-Elmer) with a 7 µL flow cell. For primary amines, phthalaldehyde and 2-mercaptoethanol (both 58 mM) in ethyl acetate were used as reagents, with detection at 431 nm (excitation at 340 nm). For secondary amines, the merged stream after reaction with the same reagents was further blended with 28 mM 7-chloro-4-nitrobenzofurazan in ethyl acetate and passed through a second 1-m coil before detection at 525 nm (excitation at 480 nm). Tertiary amines were determined by reaction with 4% malonic acid in acetic anhydride and detection at 441 nm (excitation at 400 nm). Rectilinear ranges were up to 0.8, 1.5 and 2.5 mM and coefficient of variation were 1.0, 1.3 and 2.1% for hexylamine, dihexylamine and triethylamine, respectively, as test analytes.
Fluorescence Heated reaction Review