摘要
目的:建立顶空-气相色谱法测定淫羊藿保健酒中乙醇的含量。方法:以水为溶剂,采取顶空进样,DB-WAX毛细管色谱柱(60m×0.32mm×0.25μm)测定乙醇含量。柱温为程序升温(起始温度为40℃,保持2min,以3℃·min^-1的速率升至65℃,再以50℃·min-1的速率升至200℃,保持10min);进样口温度:200℃,检测器温度:220℃。FID检测器,载气为氮气,流速10mL·mim^-1,乙醇分流比1∶1;顶空进样,进样量1000μL,顶空平衡温度85℃,平衡时间20min,定量环温度90℃,传输线温度95℃。结果:乙醇在0.000025~0.002mL·mL^-1的范围内线性关系良好,相关系数r=0.9999;仪器的精密度和方法的重复性RSD均小于5%,回收率96.7%。结论:所建立的顶空气相色谱方法准确、简单、重复性好,能够较好检测淫羊藿保健酒中乙醇的含量。
Objective: To develop a determination method of ethanol in healthcare wine by headspace GC. Method: The sample was dissolved with water and analyzed by headspace GC, with DB-WAX column (60 m×0.32 mm×0.25 μm). The temperature program for the column was as follows: initially heated at 40 ℃ for 2 min, rose to 65 ℃ at a speed of 3 ℃·min^-1 , then rose to 200 ℃ at a speed of 50 ℃·min ^-1 , lasting for 10 min;the inlet temperature was 200 ℃ and FID detector temperature was set at 220 ℃. The flow rate of the carrier gas (N 2 ) was 10 mL·mim -1 and the split ratio was 1 ∶ 1;headspace conditions were as follows: the temperature and the time of balance for the sample were 85 ℃ and 20 min, the temperature of quantitative loop and transfer lines was 90 ℃ and 95 ℃.The sample volume was 1 000 μL. Result: Linear relations was good in the reasonable rang (0.000 025 ~ 0.002 mL·mL ^-1 ), R 2 =0.999 9, the RSD of precision and repeatability of the developed method were less than 5%, and the recoveries was 96.7%, the RSD was less than 10%. Conclusion: The method is accurate, simple and repeatable, and can be used to determine the content of ethanol in herba epimedium and astragalus healthcare wine.
作者
王倩
王雪芹
朱艳春
张竞
Wang Qian;Wang Xueqin;Zhu Yanchun;Zhang Jing(Henan Provincial Institute for Food and Drug Control, Zhengzhou 450008, China)
出处
《现代食品》
2019年第20期155-159,共5页
Modern Food
关键词
保健酒
乙醇
顶空气相色谱法
内标法
Healthcare wine
Ethanol
Headspace GC
Internal standard method
