Analysis of E,E-farnesol and squalene in makgeolli using stir bar sorptive extraction coupled with gas chromatography-mass spectrometry

Abstract

The aim of this study was to establish an analytical method for the determination of E,E-farnesol and squalene in makgeolli, which is a traditional type of Korean fermented rice wine. E,E-farnesol and squalene in makgeolli were extracted using stir bar sorptive extraction (SBSE) coupled with gas chromatography-mass spectrometry. SBSE was found to be an effective method for analyzing the E,E-farnesol and squalene levels in makgeolli. The linear dynamic range of the SBSE method for detecting E,E-farnesol and squalene ranged from 0.5 to 200 ng/mL with R 2 = 0.9974 for E,E-farnesol and 100 to 50000 ng/mL with R 2 = 0.9982 for squalene.The limit of detection and the limit of quantification using the SBSE method were 0.1 and 0.5 ng/mL for E,Efarnesol and 15.0 and 40.0 ng/mL for squalene, respectively. The average recoveries obtained were, quantitatively, 101-107% for E,E-farnesol and 98-103% for squalene, respectively, supporting the accuracy of the SBSE-GCMS method.요 약: 전통주류의 한가지인 막걸리 중의 기능성 성분인 E,E-farnesol과 squalene를 분석하는 방법을 확 립하였다. 막걸리에 들어있는 E,E-farnesol과 squalene은 stir bar sorptive extraction (SBSE)와 GC-MS를 사 용 분석하였다. SBSE방법은 막걸리 중의 E,E-farnesol과 squalene함량을 분석하는데 매우 효율적이었다. 이 두 성분을 SBSE법으로 분석하였을 때 E,E-farnesol은 0.5-200 ng/mL (R 2 =0.9974) 범위에서squalene은 100-50000 ng/mL (R 2 =0.9982)에서 직선성을 보였다. SBSE법으로 분석할 경우 E,E-farnesol과 squalene의 limit of detection (LOD)와 limit of quantification (LOQ)는 각각 0.1 과 0.5 ng/mL 및 15.0과 40.0 ng/mL 이 었다. SBSE법에 의한 E,E-farnesol과 squalene의 회수율은 각각101-107%와 98-103%로 정확도가 매우 높 았다.

Simultaneous determination of four bioactive compounds in Korean rice wine (makgeolli) by solvent extraction coupled with gas chromatography-mass spectrometry

“…FOH is present at concentrations below 4 ng mL −1 in beer and wine. [9,17] The saccharification of starches in makgeolli likely provides the precursor sugars such as glucose required for the biosynthesis of FOH and SQ. [2,28] Although our SE-GC/MS method did not detect FOH or SQ in beer or wine, which may be present in very low amounts, we successfully identified measurable levels of these compounds in makgeolli samples using our newly developed method.…”

“…[16] Recently, Ha et al developed a stir-bar sorptive extraction (SBSE) method coupled with GC-MS for the quantification of FOH and SQ in makgeolli. [9,17] Although SBSE is a sensitive and selective extraction method to analyze the functional ingredients present in makgeolli, specialized equipment including a thermal desorption system is required for the GC analysis. In addition, commercial coating materials available for stir-bars (polydimethylsiloxane and ethylene glycol) limit the extraction to either nonpolar or polar compounds, but not both simultaneously.…”