title: Determination of 15 isomers of chlorobenzoic acid in soil samples using accelerated sample extraction followed by liquid chromatography.
abstract: A study was conducted to elaborate a fast, simple and efficient method for determination of 15 isomers chlorobenzoic acids (CBAs) in soil using HPLC-UV. Artificially contaminated soil samples were extracted using accelerated solvent extraction (ASE) with 1% acetic acid in a mixture of hexane and acetone (1:1, V/V) under a pressure of 10.34 MPa and temperature of 150°C. The recovery of the ASE method was above 82%. The extracts were concentrated; dimethyl sulfoxide was used to prevent CBA volatilization and the final analysis was performed with a C18 XBridge HPLC column employing a mobile phase consisting of acetonitrile and 0.1% trifluoracetic acid in water. A HPLC procedure with gradient elution and UV detection was developed and validated. The method exhibited a linear range for 2-CBA; 2,6-CBA; 3-CBA; 4-CBA; 2,3-CBA; 2,3,6-CBA; 2,5-CBA; and 2,4-CBA from 5 to 120 μg/mL with a limit of quantification (LOQ) of 5 μg/mL, RSD from 2.42 to 9.42% and accuracy from 82 ± 2 to 103 ± 3%. The linear range of determination of 2,4,6-CBA, 3,4-CBA, 2,3,5,6-CBA, 3,5-CBA, 2,3,5-CBA, 2,3,4,5,6-CBA and 2,3,4,5-CBA was 10-120 μg/mL with LOQ 10 μg/mL, RSD from 0.74 to 5.84% and accuracy from 94 ± 1 to 114 ± 1%. The optimized analytical procedure was finally applied on two historically PCB contaminated soils and 9 CBAs were quantified in the samples.
authors.affiliation: Institute of Microbiology, Academy of Sciences of Czech Republic, v.v.i., Vídeňská 1083, CZ-142 20 Prague 4, Czech Republic.
authors.forename: Zdena
authors.initials: Z
authors.lastname: Křesinová
authors.forename: Milan
authors.initials: M
authors.lastname: Muzikář
authors.forename: Jana
authors.initials: J
authors.lastname: Olšovská
authors.forename: Tomáš
authors.initials: T
authors.lastname: Cajthaml
mesh_terms: D053000:Analytic Sample Preparation Methods; D005591:Chemical Fractionation / Q000379:methods*; D002723:Chlorobenzoates / Q000032:analysis* / Q000737:chemistry / Q000302:isolation & purification*; D002851:Chromatography, High Pressure Liquid / Q000379:methods*; D007536:Isomerism; D015203:Reproducibility of Results; D012987:Soil / Q000737:chemistry*; D012989:Soil Pollutants / Q000032:analysis* / Q000737:chemistry / Q000302:isolation & purification*; D012997:Solvents / Q000737:chemistry; D013997:Time Factors
chemical_list: D002723:Chlorobenzoates; D012987:Soil; D012989:Soil Pollutants; D012997:Solvents