Abstract
The present study demonstrated the development and validation of the method for the quantification of phenol in food using gas chromatography coupled with mass spectrometry (GC-MS). After spiking of internal standard (Phenol-$d_5$) to food, those samples were extracted with organic solvent mixture (acetone : dichloromethane = 1 : 1, v/v) using ultra sonic extractor and cleaned by gel permeation chromatography (GPC) technique. The amount of phenol was determined by GC/MS. To validate the developed method, we evaluated parameters were the selectivity, linearity, accuracy, precision, and recovery. To demonstrate the selectivity of the method, blank samples of rice, corn, and fish(mackerel) were prepared and subjected to GC-MS analysis. To verify the linearity of the method, six different standard concentrations of phenol at 0.01, 0.05, 0.1, 0.5, 1 and 2.5 mg/kg were evaluated. The correlation coefficient ($r^2$) of calibration curve was 0.9999. The recovery rate for phenol standard calculated by internal standard method were 82.2~101.5% for samples fortified with 0.25, 0.50, and 1.0 mg/kg, respectively. Also the repeatability and reproducibility for validation of precision were 0.2~5.5%. According to the result of the validation, this established method was suitable for AOAC guideline. The limit of detection (LOD) for phenol analysis were 0.03~0.1 mg/kg, and the limit of quantification (LOQ) were 0.1~0.3 mg/kg. Therefore, we established the optimal analysis method for determination of phenol in food using GPC and GC/MS.
페놀은 보통 대기로 배출되며 반감기가 비교적 짧은 물질로서 환경에 농축되는 경우는 드물다. 하지만, 누출사고가 발생되어 수계나 토양에 오염될 경우 페놀에 오염된 농수산물의 안전성을 확보하기 위하여 페놀을 정확하게 검출할 수 있는 시험법을 확립하고자 하였다. 식품 중 페놀을 초음파추출기로 추출하고 GPC로 정제하여 GC/MS로 분석하는 시험법을 확립하였으며, 시험법의 유효성 확인을 위한 실험 결과들이 AOAC 가이드라인에서 제시하는 Criteria를 만족함으로써 시험법의 신뢰성을 확보할 수 있었다. 확립된 시험법은 식품 중 페놀의 오염조사 및 이행률 조사에 활용될 수 있다.
