毛细管气相色谱法测定不同干馏温度下鲜竹沥液中5-羟甲基糠醛及其衍生物的含量

Simultaneous Determination of5-Hydroxymethylfurfural and Derivatives in Xianzhuli with Different Dry Distillation Temperature by Capillary Gas Chromatography

目的建立毛细管气相色谱法测定不同干馏温度下鲜竹沥液中糠醛、2-乙基-1-己醇、5-甲基糠醛和5-羟甲基糠醛的含有量。方法采用DB-WAX色谱柱,FID检测器,进样口温度:250℃;程序升温:初始温度65℃,保留0.5 min,3℃·min^(-1)升至120℃保留0.5 min,8℃·min^(-1)升至230℃,280℃后运行8 min;N2为载气,柱流速:3.5 mL·min^(-1),进样1μL分流比10∶1;FID检测器温度300℃。结果糠醛、2-乙基-1-己醇、5-甲基糠醛和5-羟甲基糠醛在范围内线性关系良好(R^(2)≥0.999 7),平均回收率为≥95.08%,RSD为≤2.16%。结论该方法准确稳定,重复性好,可为鲜竹沥的工艺参数以及质量控制提供参考。

OBJECTIVE To establish a capillary gas chromatography method for the determination of furfural,2-ethyl-1-hexanol,5-methylfurfural,5-hydroxymethylfurfural in Xianzhuli with different dry distillation temperature.METHODS The analysis of Xianzhuli solution was performed on a DB-WAX capillary column(30 m×0.32 mm,0.25 μm) with FID as the detector,the initial temperature was65℃(keeping 0.5 minutes),with 3 ℃·min^(-1) to 120 ℃(keeping 0.5 minutes),with 8 ℃·min;to 230 ℃;280 ℃(post run 8 minutes).The FID detector temperature was 300 ℃ and the injector temperature was 250 ℃,The carrier gas was N2(99.999%) with the flow rate at 3.5 mL·min^(-1).The sample volume was 1 μL,and the split ratio was 10:1.RESULTS The furfural,2-ethyl-1-hexanol,5-methylfurfural and 5-hydroxymethylfurfural showed good linear relationships(R^(2)≥0.999 7),average recoveries≥95.04%,with the RSD of≤2.16%.CONCLUSION This accurate,stable and reprod ucible method can provide reference for the technological parameter and quality control of Xianzhuli.