气相色谱法测定食品添加剂柠檬酸脂肪酸甘油酯中柠檬酸的改进

Improvement of the method for determination of citric acid in citric acid fatty acid glyceride by gas chromatography

中文关键词:  气相色谱法  总柠檬酸  添加剂

英文关键词:gas chromatography  citric acid  additive

中文摘要:

      目的 改进气相色谱法测定食品添加剂柠檬酸脂肪酸甘油酯中柠檬酸的分析方法。方法 对测定食品添加剂柠檬酸GB 29951-2013《食品安全国家标准 食品添加剂 柠檬酸脂肪酸甘油酯》的气相色谱法中衍生剂、色谱柱以及升温程序进行优化, 并对优化后的方法进行验证。结果 选择N,O-双(三甲基硅烷基)-三氟乙酰胺(BSTFA)作为衍生剂, HP-5毛细管柱作为分离柱, 温度程序为80 ℃(1 min) 20 ℃/min165 ℃(5 min) 30 ℃/min250 ℃(1 min), 可在15 min内完成对目标物的分离, 线性方程为Y=0.67193X+0.05490, r=0.9935, 方法回收率为93.0%~98.7%, 相对标准偏差(relative standard deviation, RSD)为0.4%, 检出限为0.1%。结论 该方法目标物分离效果好, 回收率及灵敏度高, 适用于食品添加剂柠檬酸的定量检测。

英文摘要:

      Objective To improve gas chromatography method for the determination of citric acid in glyceryl citrate fatty acid ester of food additive. Methods According to GB 29951-2013 National food safety standard-Food safety national standard food additive extraction method of citric acid fatty acid glyceride, the derivative, column and temperature program for gas chromatography were optimized, and the optimized method was verified. Results BSTFA was selected as a derivative agent, HP-5 capillary column was selected as a separation column, the temperature procedures was 80 ℃ (1 min) 20 ℃/min 165 ℃ (5 min) 30 ℃ / min 250 ℃ (1 min). The separation of the target object could be completed within 15 min. The linear equation was Y=0.67193X+0.05490, r=0.9935. The recovery rate of the method was between 93.0% and 98.7%, and the relative standard deviation (RSD) was 0.4%, detection limit was 0.1%. Conclusion The method has good separation effect, high recovery and sensitivity, and is suitable for quantitative determination of citric acid in food additives