液液萃取-气相色谱法测定黄酒中β-苯乙醇含量

Determination of β-Phenylethanol in Chinese Rice Wine by LiquidLiquid Extraction-Gas Chromatography

建立黄酒中β-苯乙醇的液-液萃取-气相色谱检测方法,为炮制辅料黄酒的质量控制研究提供参考。用碳酸钠饱和的15%乙醇溶液与乙酸乙酯1︰1 (V/V)混合均匀,超声分层,取上层澄清液作为萃取剂;采用气相色谱法,Agilent HP-5色谱柱(30 m×0.32 mm×0.25μm), FID检测器,进样口温度230℃,检测器温度250℃,柱温程序升温为:初始温度120℃,恒温2 min,以25℃/min升温至210℃,恒温10 min,柱流量1 mL/min,进样量1.0μL,内标物4-(4-甲氧苯基)-2-丁酮。结果表明,β-苯乙醇在4.86～243.02 mg/L范围内线性关系良好(r=0.999 9),精密度试验RSD值为0.20%,重复性试验RSD值为4.66%, 3种加标浓度的回收率在94.28%～102.57%之间,检出限为0.08 mg/L,定量限为0.20mg/L。该方法具有简单、可靠、结果准确等优点,同时有效降低黄酒中糖分、色素等基质对气相色谱系统的污染,减少水分对毛细管色谱柱的危害,可用于辅料黄酒中β-苯乙醇含量检测及质量控制。

To establish a method for the determination ofβ-phenylethanol in Chinese rice wine by liquid-liquid extraction-gas chromatography(GC),a reference for the quality control of processed rice wine was provided.The 15%ethanol solution saturated with sodium bicarbonate was mixed with ethyl acetate in the ratio of 1︰1(V/V)evenly and the upper clarification solution was used as extractant.The GC was performed on Agilent HP-5 column(30 m×0.32 mm×0.25μm)with a flame ionization detector(FID).The injector temperature was 230℃and detector temperature was set at 250℃.The temperature program of column oven was set as follows:120℃for 2 min,increased to 210℃at the rate of 25℃/min.The injection volume was set as 1.0μL with a flow rate of 1 mL/min and 4-(4-methoxyphenyl)-2-butanone was used as internal standard.Results showed that theβ-phenylethanol was in good linear correlation in the concentration rang of 4.86-243.02 mg/L(r=0.9999).The mean recovery(n=9)was between 94.28%and 102.57%.The method could effectively reduce the pollution from rice wine matrix such as sugar and pigment on gas chromatography system and the harm of capillary column from water content in rice wine samples,and it was simple,reliable,accurate and applicable to the determination and the quality control ofβ-phenylethanol in rice wine.