Single-drop microextraction with in-microvial derivatization for the determination of haloacetic acids in water sample by gas chromatography-mass spectrometry.

摘要: Abstract A new approach using single-drop microextraction (SDME) and gas chromatography–mass spectrometry for the determination of six haloacetic acids (HAAs) in water samples was presented. n -Octanol used as extractant derivatization reagent. HAAs were derivatized both simultaneously during extraction solvent microdrop, after extraction, inside a glass microvial (1.1 mm I.D.). Trifluoroacetic anhydride (TFAA) reaction catalyst. The influence catalyst amount, time temperature on yield in-microvial investigated. Derivatization performed 1.2 μL TFAA at 100 °C 20 min. Extraction 1.8 μL -octanol containing (10%, v/v). Experimental parameters, such as, exposure time, sample pH controlled optimized. Analytical parameters linearity, precision limit detection also evaluated. proposed method proved to be suitable analytical procedure with limits 0.1–1.2 μg/L. relative recoveries range from 82.5 97.6% all target analytes. Precision values 5.1 8.5% (as intra-day standard deviation, RSD) 8.8–12.3% inter-day RSD).