Journal
JOURNAL OF CHROMATOGRAPHY A
Volume 1352, Issue -, Pages 8-19Publisher
ELSEVIER SCIENCE BV
DOI: 10.1016/j.chroma.2014.05.061
Keywords
Ultrasonic-assisted derivatization; microextraction (UDME); 1-(1H-imidazol-1-yl)-2-(2-phenyl-1H-phenanthro[9,10-d]imidazol-1-yl)ethanone (IPPIE); Aliphatic amines; Environmental samples; UDME-HPLC-FD-MS
Funding
- Natural Science Foundation of Shandong Province, China [ZR2013BQ019]
- 100 Talents Program of The Chinese Academy of Sciences [328]
- National Natural Science Foundation of China (General Program) [21275089]
- Key Laboratory of Bioorganic Analysis Shandong Province, Key Laboratory of Pharmaceutical Intermediates and Analysis of Natural Medicine Shandong Province [XJ201102]
- Qufu Normal University, and the undergraduate research-training programs [2011A026]
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A new fluorescent reagent, 1-(1H-imidazol-1-yl)-2-(2-pheny1-1H-phenanthro[9,10-d]imidazol-1-yl]ethanone (IPPIE), is synthesized, and a simple pretreatment based on ultrasonic-assisted derivatization microextraction (UDME) with IPPIE is proposed for the selective derivatization of 12 aliphatic amines (C-1: methylamine-C-12: dodecylamine) in complex matrix samples (irrigation water, river water, waste water, cultivated soil, riverbank soil and riverbed soil). Under the optimal experimental conditions (solvent: ACN-HCl, catalyst: none, molar ratio: 43, time: 8 min and temperature: 80 C), micro amount of sample (40 mu L; 5 mg) can be pretreated in only 10 min, with no preconcentration, evaporation or other additional manual operations required. The interfering substances (aromatic amines, aliphatic alcohols and phenols) get the derivatization yields of <5%, causing insignificant matrix effects (<4%). IPPIE-analyte derivatives are separated by high performance liquid chromatography (HPLC) and quantified by fluorescence detection (FD). The very low instrumental detection limits (IDL: 0.66-4.02 ng/L) and method detection limits (MDL: 0.04-033 ng/g; 5.96-45.61 ng/L) are achieved. Analytes are further identified from adjacent peaks by on-line ion trap mass spectrometry (MS), thereby avoiding additional operations for impurities. With this UDME-HPLC-FD-MS method, the accuracy (-0.73-2.12%), precision (intra-day: 0.87-3.39%; inter-day: 0.16-4.12%), recovery (97.01-104.10%) and sensitivity were significantly improved. Successful applications in environmental samples demonstrate the superiority of this method in the sensitive, accurate and rapid determination of trace aliphatic amines in micro amount of complex samples. (C) 2014 Elsevier B.V. All rights reserved.
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