Development of heat-assisted in-situ solvent formation liquid phase microextraction followed by derivatization for the simultaneous extraction of aliphatic amines from wastewater samples prior to gas chromatography-mass spectrometry

Abstract

Herein, a cost-effective, rapid, and selective liquid phase microextraction procedure has been developed for the extraction of some aliphatic amines from sewage samples. The method was based on in-situ formation of chloroform as an extraction solvent into the sample solution followed by derivatization by butylchloroformate prior to gas chromatography- mass spectrometry. Chloroform is formed by the reaction of chloral hydrate and sodium hydroxide. The extraction procedure was accelerated by heating. Also heating decreases chloroform solubility in aqueous solution. To improve the analytical signals, derivatization of the analytes is done by butylchloroformate. The effect of major parameters on the extraction efficiency were studied and optimized. Under the optimized conditions, enrichment factor and extraction recovery were in the ranges of 259–296 and 78–89 %, respectively. Low limits of detection (0.08–0.12 ng mL−1) and quantification (0.28–0.41 ng mL−1), wide linear ranges, and relative standard deviations less than 6 % for intra −and inter-day precisions were acceptable. Lastly, the mentioned method was successfully performed to determine aliphatic amines in wastewater samples.