Abstract: An improved reagent named 2-[2-(dibenzocarbazole)-ethoxy] ethyl chloroformate (DBCEC-Cl) for the determination of aliphatic amines by high-performance liquid chromatography (HPLC) with fluorescence detection and post-column online atmospheric chemical ionization-mass spectrometry (APCI-MS) identification has been developed. DBCEC-Cl could easily and quickly label aliphatic amines. Derivatives were stable enough to be efficiently analyzed by HPLC and showed an intense protonated molecular ion corresponding m/z [M+H]+ under APCI-MS in positive-ion mode. The ratios for fluorescence responses were IDBCEC-amine/IBCEC-amine = 1.02–1.60; IDBCEC-amine/IBCEOC-amine = 1.30–2.57; and IDBCEC-amine/IFMOC-amine = 2.20–4.12 (here, I was relative fluorescence intensity). The ratios for MS responses were ICDBCEC-amine/ICBCEC-amine = 4.16–29.31 and ICDBCEC-amine/ICBCEOC-amine = 1.23–2.47 (Here, IC: APCI-MS ion current intensity). Detection limits calculated from 0.0244 pmol injection, at a signal-to-noise ratio of 3, were 0.3–3.0 fmol. The relative standard deviations for within-day determination (n = 6) were 0.045–0.081% for retention time and 0.86–1.03% for peak area for the tested aliphatic amines. The mean intra- and inter-assay precision for all amine levels were <3.64% and 4.67%, respectively. The mean recoveries ranged from 96.9% to 104.7% with their standard deviations in the range of 1.80–2.70 (RSDs%). Excellent linear responses were observed with coefficients of >0.9991.

Jinmao You, Cuihua Song, Tao Yan, Zhiwei Sun, Yulin Li, Yourui Suo. An improved reagent for determination of aliphatic amines with fluorescence and online atmospheric chemical ionization-mass spectrometry identification. Analytica Chimica Acta, 2010, 65: 898–105

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