[Determination of aliphatic amines by high performance liquid chromatography with fluorescence and atmospheric pressure chemical ionization detection and identification by mass spectrometry].
Aliphatic amines exist widely in nature. Therefore, quick and precise determination of aliphatic amines is of great significance. A simple and highly sensitive method based on the derivatization of aliphatic amines utilizing 1,2-benzo-3,4-dihydrocarbazole-9-acetic acid (BCAA) as the novel pre-column derivatization reagent followed by high performance liquid chromatography with fluorescence detection and online mass spectrometric identification was developed. Optimum derivatization was obtained by the reaction of aliphatic amines with BCAA at 50 degrees C for 15 min in the presence of 1-ethyl-3-(3-dimethyl aminopropyl) carbodiimide (EDAC) in acetonitrile solvent. The condition of derivatization was mild and the yield of derivative each aliphatic amine was higher than 94%. Derivatives were sufficiently stable to be efficiently analyzed by high performance chromatography without pretreatment. On a reversed-phase BDS-C18 column, twelve aliphatic amine derivatives (C8 - C12) were separated under gradient elution with baseline resolution. The precise determining aliphatic amines from soil and wastewater samples was obtained by post-column online mass spectrometric identification with atmospheric pressure chemical ionization (APIC) source under positive mode detection. The established method exhibited excellent reproducibility and recovery. Linear responses were observed with coefficients over 0.999 3. The detection limits (at signal-to-noise ratio of 3: 1) were 12 - 28 fmol.
College of Chemistry Science, Qufu Normal University, Qufu 273165, China. xmch913@163.com
Xiangming
X
Chen
Yunwei
Y
Shi
Xian'en
X
Zhao
Haifeng
H
Zhang
Jinmao
J
You
D000097:Acetonitriles / Q000737:chemistry; D000588:Amines / Q000032:analysis* / Q000737:chemistry; D002234:Carbodiimides / Q000737:chemistry; D002851:Chromatography, High Pressure Liquid / Q000379:methods*; D013058:Mass Spectrometry / Q000379:methods*; D015203:Reproducibility of Results; D012989:Soil Pollutants / Q000032:analysis / Q000737:chemistry; D013050:Spectrometry, Fluorescence / Q000379:methods*; D014874:Water Pollutants, Chemical / Q000032:analysis / Q000737:chemistry
D000097:Acetonitriles; D000588:Amines; D002234:Carbodiimides; D012989:Soil Pollutants; D014874:Water Pollutants, Chemical; C074139:1-ethyl-3-(3-dimethylaminoethyl)carbodiimide; C032159:acetonitrile