Headspace solid-phase microextraction applied to the simultaneous determination of sorbic and benzoic acids in beverages Original Research Article

A new analytical procedure was developed using headspace solid-phase microextraction (HS-SPME) for the simultaneous determination of sorbic and benzoic acids in beverages. The sample were processed depending on their nature, either only diluted with water, or treated with a NaOH solution and filtered through a 0.45-μm membrane filter. The samples were heated in a vial in the presence of sulfuric acid and anhydrous sodium sulfate and the analytes were collected from the headspace by using a 65-μm polydimethylsiloxane–divinylbenzene (PDMS–DVB) coated fiber and determined by gas chromatography with flame ionization detector (GC-FID). To enhance the sensitivity of HS-SPME, the temperature and time of the extraction and desorption, the acidity and salt concentration of the extraction solution were optimized. Linear range of the analytes was found to be between 0.1 and 20 mg/L with regression coefficients (R2) of 0.9998 for sorbic acid and 0.9980 for benzoic acid. Limits of detection (LOD) were 5.83 μg/L and 11.4 μg/L for sorbic and benzoic acids, respectively. Relative standard deviation (R.S.D.) for six replicate analyses within 3 days (two times/day) was found to be lower than 8.62% at three concentration levels (2, 6, 10 mg/L). Recoveries ranged from 81.20% to 108.1% for real samples. The results demonstrate the suitability of the HS-SPME technique to analyze sorbic and benzoic acids in a variety of beverages.