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

Abstract

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 μm (PA). The best extraction conditions were as follows: 200 μL of derivatizing agent (acetic anhydride), 20 mL of saturated aqueous NaCl solution and extraction time and temperature of 50 min and 75°C, respectively. All optimized conditions were obtained with fixed leather sample mass (250 mg), vial volume (40 mL) and phosphate buffer pH (12) and concentration (50 mmol/L). Detection limits ranging from 0.03 to 0.20 ng/g, and relative standard deviation (RSD) lower than 10.23% (n=6) for a concentration of 800 ng/g (chlorophenols) and 1325 ng/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.

Determination of organochlorine pesticides in leather by solid-phase microextraction and gas chromatography-mass spectrometry

“…The results of this study, shown in Figure 2, indicate a reduction in the extraction efficiency of the OCPs when the ionic strength was increased. This finding is in agreement with that reported by Dong [7] , Prates [8] and Pawliszyn [9,10,11] who studied the salting out effect on the extraction of OCPs. Therefore, no salt was added to the vials for the next steps of this study.…”

Characterization of Cultivar Differences of Blueberry Wines Using GC-QTOF-MS and Metabolic Profiling Methods

“…It has been demonstrated that LiChrolut-EN has a much stronger retention of volatiles than other commonly used sorbents, such as bond Elut ENV (styrene- divinylbenzene), Amberlite, and Tenax TA [ 20 , 21 ]. Another commonly used technique is solid phase microextraction (SPME), which can extract volatile and semi-volatile organic compounds from environmental, biological, and food samples [ 22 , 23 , 24 ]. There are also a lot of commercially available stationary phases, although the divinylbenenze/carboxen/polydimethylsiloxane (DVB/CAR/PDMS) is the most frequently used on an expanded range of analytes.…”

Ultrasound‐assisted dispersive micro‐solid‐phase extraction using hydrophobic thiolated ionic liquids immobilized on gold nanoparticles for the preconcentration and determination of amino acids in human plasma samples

“…Generally, application of one‐variable‐at‐a‐time optimization method has some disadvantages, including tediousness and inability to predict interaction among factors. Experimental design (full or fractional factorial design) have been used for optimization of microextraction methods and prediction of the main and interaction effects . Based on the preliminary studies, six variables including amount of adsorbent, eluent volume, ultrasound time, ionic strength, desorption time and aqueous sample volume were considered.…”