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PH12 Analytical Environmental Chemistry of POPs
(PH130) Trace determination of 1-aminopropanone, a marker for wastewater contamination, by liquid chromatography with fluorescence detection (LC-FL).
Singh, Simrat1, Gardinali, Piero2, 1 Graduate student,chemistry dept, Florida international University, Miami, Florida, USA2 Assistant Proffesor, chemistry department,Florida international university, Miami, Florida, USA
ABSTRACT- 1-Aminopropanone (APR) is a volatile aminoketone of human origin that has been identified in raw sewage and surface waters. It is a minor component of urine, as an average person excretes about 0.4mg of aminopropanone each day. Aminopropanone is form in the body by condensation of glycine with acetyl co- enzyme- A and by oxidation of threonine. The half- life of APR is about 8-9 days in raw sewage. Hence, It could be used as a valuable marker for raw sewage intrusions in coastal systems served by septics like the Florida Keys. The traditional methodology for the determination of APR is extremely complicated and not very sensitive. The first reported method method involved pre-concentration of water samples by purging the volatile amines, formation of the hydrochloride, derivatization and GC/MS analysis. Further developments included the incorporation of in-line derivatization on a C-18 cartridge containing DNPH. Although these changes enhanced the reproducibility of the determination the protocol is still tedious and requires a skilled chemist to achieve good results. This investigation presents a novel and simple method for the detection of aminopropanone by direct derivatization in aqueous media followed by HPLC detection. This method involves water based reaction.The reagents used are o-Pthalaldehyde and mercaptoethanol.The reaction is maintained at a pH of 9.5 by adding sodium borate, which helps in the deprotonation of APR. The reaction is time dependent and measurements should be conducted between 5 and 15 minutes. The highly fluorescent product of this reaction is separated on a 15 cm x 4.6 mm Luna C-18 column (1 ml/min, 50:10 Methanol: Water) and detected using an excitation and emission wavelengths of 350 nm and 455 nm respectively. Limits of detection in the 50 parts per trillion (ng/L) range can be achieved by concentrating and analyzing a 1 liter water sample.
Key words: Aminopropanone
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