title: Single-drop microextraction with in-microvial derivatization for the determination of haloacetic acids in water sample by gas chromatography-mass spectrometry.
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 was used as extractant and derivatization reagent. HAAs were derivatized both simultaneously during the extraction in the solvent microdrop, and after extraction, inside a glass microvial (1.1mm I.D.). Trifluoroacetic anhydride (TFAA) was used as the reaction catalyst. The influence of catalyst amount, derivatization time and temperature on the yield of the in-microvial derivatization was investigated. Derivatization reaction was performed using 1.2microL of TFAA at 100 degrees C for 20min. Extraction was performed using 1.8microL of n-octanol containing TFAA (10%, v/v). Experimental parameters, such as, exposure time, sample pH and extraction temperature were controlled and optimized. Analytical parameters such as linearity, precision and limit of detection were also evaluated. The proposed method was proved to be a suitable analytical procedure for HAAs in water with limits of detection 0.1-1.2microg/L. The relative recoveries range from 82.5 to 97.6% for all the target analytes. Precision values were from 5.1 to 8.5% (as intra-day relative standard deviation, RSD) and 8.8-12.3% (as inter-day RSD).
authors.affiliation: Department of Chemistry, Isfahan University of Technology, Isfahan 84156-83111, Iran. saraji@cc.uit.ac.ir
authors.forename: Mohammad
authors.initials: M
authors.lastname: Saraji
authors.forename: Ali Akbar Hajialiakbari
authors.initials: AA
authors.lastname: Bidgoli
mesh_terms: D020003:1-Octanol / Q000737:chemistry; D000085:Acetates / Q000032:analysis*; D001966:Bromine / Q000032:analysis*; D005591:Chemical Fractionation / Q000379:methods*; D002713:Chlorine / Q000032:analysis*; D005618:Fresh Water / Q000737:chemistry; D008401:Gas Chromatography-Mass Spectrometry / Q000379:methods*; D006863:Hydrogen-Ion Concentration; D015203:Reproducibility of Results; D012680:Sensitivity and Specificity; D012997:Solvents / Q000737:chemistry; D013431:Sulfates / Q000737:chemistry; D013696:Temperature; D014269:Trifluoroacetic Acid / Q000737:chemistry; D014877:Water Pollution, Chemical / Q000032:analysis*
chemical_list: D000085:Acetates; D012997:Solvents; D013431:Sulfates; C012036:sodium sulfate; D002713:Chlorine; D014269:Trifluoroacetic Acid; D020003:1-Octanol; D001966:Bromine