Application of solid-phase microextraction and gas chromatography-mass spectrometry for the determination of chlorophenols in leather

This paper proposes a new analytical procedure based on the headspace solid-phase microextraction (HS-SPME) technique and gas chromatography-selected ion monitoring-mass spectrometry (GC-SIM-MS) for the determination of 16 phenols extracted from leather samples. The optimized conditions for the HS-SPME were obtained through two experimental designs a two-level fractional factorial design followed by a central composite design using the commercial SPME fiber polyacrylate 85 mu m (PA). The best extraction conditions were as follows: 200 mu L of derivatizing agent (acetic anhydride), 20mL of saturated aqueous NaCl solution and extraction time and temperature of 50min and 75 degrees C, respectively. All optimized conditions were obtained with fixed leather sample mass (250mg), vial volume (40mL) and phosphate buffer pH (12) and concentration (50mmol/L). Detection limits ranging from 0.03 to 0.20ng/g, and relative standard deviation (RSD) lower than 10.23% (n=6) for a concentration of 800ng/g (chlorophenols) and 1325ng/g (2-phenylphenol) in the splitless mode were obtained. The recovery was studied at three concentration levels by adding different amounts of phenols to the leather sample and excellent recoveries ranging from 90.0 to 107.2% were obtained. The validated method was shown to be suitable for the quantification of phenols in leather samples, as it is simple, relatively fast and sensitive.