Use of Sorbent-Based Vacuum Extraction for Determination of Volatile Phenols in Beer
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Use of Sorbent-Based Vacuum Extraction for Determination of Volatile Phenols in Beer Henryk H. Jeleń 1 & Anna Gaca 1 & Monika Marcinkowska 1 Received: 13 February 2018 / Accepted: 23 April 2018 # The Author(s) 2018
Abstract A novel method based on vacuum-assisted sorbent extraction (VASE) used with gas chromatography-mass spectrometry (GCMS) for isolation of volatile phenols was described. The method is based on extraction of analytes into sorbent traps (sorbent pen) filled with Tenax in a vacuum system—vials with traps from which air was evaluated. The method was applied for extraction of volatile phenols from aqueous matrix and smoked beer was used as a food example. Methyl-, dimethyl-, and trimethylphenols, along with 4-ethylphenol, 4-methylguaiacol, 4-ethylguaiacol, 4-propylguaiacol, and eugenol, were used in method development. Optimal extraction parameters were elaborated. For the analysis of volatile phenols in beer matrix, the method was characterized with satisfactory linearity (r2 ≥ 0.99) in a range of 0.005–0.5 mg/L. Limits of detection (LODs) for analyzed compounds ranged from 0.0006 to 0.018 mg/L and repeatability for majority of compounds was < 5% for a single trap extraction. The detected volatile phenols in beer samples ranged from 0.003 to 0.672 mg/L. Keywords Vacuum-assisted sorbent extraction . VASE . Volatile phenols . Beer
Introduction For the analysis of food flavor compounds, numerous extraction techniques are used (Augusto et al. 2003). Headspace analysis allows the determination of volatile compounds from simple liquid, as well as complex, often non-homogenous matrices. Though static headspace is the simplest extraction technique, it offers no preconcentration step and usually is characterized by relatively low sensitivity. Therefore, more popular are extraction techniques based on sorbents, especially in microscale (Baltussen et al. 2002). Among them, solid-phase microextraction (SPME) gained the highest popularity due to the method robustness, sensitivity, selectivity based on partition constants, and integration of extraction and preconcentration in one device that also allows the simple sample transfer to gas chromatograph (Jeleń et al. 2012). Headspace SPME is highly suitable for compounds that have high Henry’s law volatility constant (KH). However, compounds which are characterized with low KH, for which gas-phase resistance controls more than
* Henryk H. Jeleń [email protected] 1
Faculty of Food Science and Nutrition, Poznań University of Life Sciences, Wojska Polskiego 31, 60-624 Poznań, Poland
95% of the evaporation rate (Psillakis et al. 2012; Psillakis 2017), are not favored in SPME extraction. Usually, in water matrices, polar compounds of low volatility are the most difficult to analyze by SPME. The effect of vacuum on SPME extraction was noted for the first time by Brunton and coworkers (Brunton et al. 2001), who noticed improved extraction efficiency when using Carboxen/PDMS fiber to extract volatile compounds from a cooked and raw turkey breast. A rotary vane p
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