气相色谱法测定食糖中二十八烷醇含量

Determination of octacosanol in sugar by gas chromatography

中文关键词:  二十八烷醇  食糖  气相色谱法

英文关键词:octodecanol  sugar  gas chromatography

中文摘要:

      目的 建立气相色谱法检测食糖中二十八烷醇含量的分析方法。方法 将食糖样品用蒸馏溶解, 加入乙酸乙酯提取后进行减压蒸馏浓缩, 将浓缩提取液用HP-5 (30 m×320 μm, 0.25 μm)毛细管色谱柱分离, 用气相色谱仪检测, 外标法进行定量。结果 二十八烷醇标准曲线在质量浓度10~100 mg/L区间内呈现良好的线性关系, 得出的相关系数(r2)大于0.9999; 方法检出限(S/N=3)为0.048 mg/kg, 定量限(S/N=10)为0.16 mg/kg; 应用不同类型的食糖样品进行实验分析, 红糖二十八烷醇含量较其他类食糖高; 分别在样品中添加二十八烷醇标准溶液, 进行3水平(2、10、20 mg/kg)添加回收实验, 平均回收率为94.7%~103.3%, 相对标准偏差为1.73%~3.56%。结论 该方法样品制备简单, 准确性、重现性和回收率均符合常规检测的需要, 适用于食糖样品中二十八烷醇含量的测定。

英文摘要:

      Objective To establish a method for the determination of octacosanol in sugar by gas chromatography. Methods The sugar samples were dissolved by distillation, extracted by adding ethyl acetate, and concentrated by distillation under reduced pressure. The concentrated extract was separated by HP-5 (30 m× 320 μm, 0.25 μm) capillary column, detected by gas chromatograph, and quantified by external standard method. Results The standard curve of octacosanol showed a good linear relationship in the mass concentration range of 10–100 mg/L, and the correlation coefficient (r2) was greater than 0.9999; the detection limit of the method (S/N=3) was 0.048 mg/kg, and the limit of quantification (S/N=10) was 0.16 mg/kg. Using different types of sugar samples for experimental analysis, it was found that the octacosanol content of brown sugar was higher than other kinds of sugar; the standard solution of octacosanol were added to the samples separately, conducting 3 level (2, 10, 20 mg/kg) fortification recovery test, the average recoveries were 94.7%–103.3%, and the relative standard deviations were 1.73%–3.56%. Conclusion The method is simple to prepare, the accuracy, reproducibility and recovery rate meet the needs of routine detection, and is suitable for the determination of the content of octacosanol in sugar samples.