Application of modified hollow fiber liquid phase microextraction in conjunction with chromatography-electron capture detection for quantification of acrylamide in waste water samples at ultra-trace levels

- Modified hollow fiber liquid phase microextraction.
- GC-ECD and GC-MS detection.
- High clean up and efficient sample preparation method.
- Appropriate pre-concentration factor and method detection limit.
- Acrylamide.
- Waste water samples.

Herein, a simple and sensitive method was successfully developed for the extraction and quantification of acrylamide in water samples. Initially, acrylamide was derivatized through a bromination process. Subsequently, a modified hollow-fiber liquid-phase microextraction was applied for the extraction of the brominated acrylamide from a 10-ml portion of an aqueous sample. Briefly, in this method, the derivatized acrylamide (2,3-dibromopropionamide) was extracted from the aqueous sample into a thin layer of an organic solvent sustained in pores of a porous hollow fiber. Then, it was back-extracted using a small volume of organic acceptor solution (acetonitril, 25 μl) located inside the lumen of the hollow fiber followed by gas chromatography-electron capture detection (GC-ECD). The optimal conditions were examined for the extraction of the analyte such as: the organic solvent: dihexyl ether + 10% tri-n-octyl phosphine oxide; stirring rate: 750 rpm; no salt addition and 30 min extraction time. These optimal extraction conditions allowed excellent enrichment factor values for the method. Enrichment factor, detection limit (S/N = 3) and dynamic linear range of 60, 2 ng L−1 and 50-1000 ng L−1 to be determined for the analyte. The relative standard deviations (RSD%) representing precision of the method were in the range of 2.2-5.8 based on the average of three measurements. Accuracy of the method was tested by the relative recovery experiments on spiked samples, with results ranging from 93 to 108%. Finally, the method proved to be simple, rapid, and cost-effective for routine screen of acrylamide-contaminated highly-complicated untreated waste water samples.