固相萃取-气相色谱法测定黄酒中β-苯乙醇含量

目的:建立黄酒中β-苯乙醇的固相萃取-气相色谱检测方法。方法:HLB型固相萃取小柱经活化、平衡后,对3.0 mL黄酒样品中的β-苯乙醇进行富集,依次以3.0 mL水、3.0 mL体积分数40%甲醇溶液淋洗小柱,用3.0 mL甲醇洗脱样品,用气相色谱-氢火焰离子化检测器对目标物进行检测,外标法定量。结果:β-苯乙醇在10.1~202.0 mg/L质量浓度范围内,线性相关系数(r)为0.999 9,检出限(RSN=3)和定量限(RSN=10)分别为0.9 mg/L和3.0 mg/L,回收率在95.5%~98.5%之间,相对标准偏差为1.1%~1.4%。结论:该方法具有操作便捷、结果准确的优点,同时有效降低了黄酒基质对气相色谱系统的污染,避免了酒样中水分对毛细管色谱柱的危害,适用于黄酒中β-苯乙醇的检测。

Determination of β-Phenylethanol in Rice Wine by Solid Phase Extraction-Gas Chromatography

Objective: To establish a method for the determination of β-phenylethanol in rice wine by solid phase extraction (SPE)-gas chromatography (GC). Methods: β-Phenylethanol was enriched from 3.0 mL of rice wine with an activated and balanced HLB solid phase extraction column, which was washed with 3.0 mL of water and 3.0 mL of methanol-water (4:6, V/V), and eluted with 3.0 mL of methanol. A gas chromatograph equipped with flame ionization detector (GC-FID) was used to analyze the target compounds. Results: In the concentration range of 10.1–202.0 mg/L, good linearity was achieved with a correlation coefficient (r) of 0.999 9. The limit of detection (LOD, RSN = 3) and the limit of quantification (LOQ, RSN = 10) were 0.9 and 3.0 mg/L, respectively. The recovery of β-phenylethanol was in the range of 95.5%?98.5%. The precision values expressed as relative standard deviations (RSDs) were 1.1%?1.4%. Conclusion: The method is simple, convenient, accurate and applicable to the determination of β-phenylethanol in rice wine and can effectively reduce the pollution of the gas chromatography system by rice wine matrix and prevent water in rice wine samples from bringing harm to the capillary column.