固液分散萃取-高效液相色谱法测定蜂蜜中甘油残留量

Determination of glycerin residue in honey by high performance liquid chromatography with dispersive solid-liquid-phase extraction method

中文关键词:  蜂蜜  甘油  高效液相色谱法  快速检测  质量控制

英文关键词:honey  glycerin  high performance liquid chromatography  rapid determination  quality control

中文摘要:

      目的 建立固液分散萃取-高效液相色谱法测定蜂蜜中甘油残留量的方法。方法 样品经乙醇溶解, 用微粉硅胶吸附, 使蜂蜜均匀分散成细微颗粒。水浴蒸干水分和乙醇, 以乙腈为溶剂超声萃取, 样液用带示差折光检测器的高效液相色谱仪测定。采用Shodex Asahipak NH2P-50 4E色谱柱分离, 以赤藓糖醇为内标, 以阴性样品为基质绘制标准曲线进行内标法定量, 流速为1.0 mL/min, 流动相为乙腈水溶液。结果 此方法能在6.5 min内快速分离甘油, 甘油在50~1000 mg/kg范围内线性良好, 相关系数r2=0.9996。甘油回收率为94.8%~102.9%, 相对标准偏差为2.9%~5.3%。结论 该方法具有简单、快速、灵敏度高等特点, 可用于蜂蜜中甘油的检测。

英文摘要:

      Objective To establish a method for the determination of glycerin residue in honey by high performance liquid chromatography with dispersive solid-liquid-phase extraction method. Methods The sample was dissolved by ethanol and absorbed by micro silica gel to disperse honey into fine particles. The water and ethanol was evaporated using water bath. The glycerin in honey was extracted by ultrasonic using acetonitrile as solvent. Then the honey samples are analyzed by the HPLC column Shodex Asahipak NH2P-50 4E with the total flow rate 1.0 mL/min. Internal standard method was used to quantify the standard curve with erythritol as the internal standard and negative sample as the matrix. The mobile phase was acetonitrile aqueous solution. Results The glycerin could be effectively separated in 6.5 min. The linearity of glycerol ranged from 50 to 1000 mg/kg and the correlation coefficient was 0.9996. The recovery rate ranged from 94.8% to 102.9% and the relative standard deviation was 2.9% to 5.3%. Conclusion This method is simple, rapid, sensitive to provide a new insight for the daily determination of glycerin in honey.