高效液相色谱法同时测定加工食品中5种添加剂含量

Simultaneous determination of 5 kinds of additives content in processed food by high performance liquid chromatography

中文关键词:  食品添加剂  梯度洗脱  同时测定  高效液相色谱法

英文关键词:food additives  gradient elution  simultaneous determination  high performance liquid chromatography

中文摘要:

      目的 建立高效液相色谱法同时测定加工食品中苯甲酸、山梨酸、糖精钠、脱氢乙酸、纳他霉素5种添加剂含量的分析方法。方法 通过优化梯度洗脱程序、流动相pH、柱温等参数, 确定最佳分析条件。参照国家标准方法进行样品前处理, 以加标方式考察该分析方法的线性范围、定量限、检出限、准确度、精密度、基质适应性等方法学指标。结果 5种添加剂在各浓度范围内线性关系良好, 相关系数(r2)均大于0.999; 检出限(S/N=3)分别为: 苯甲酸、山梨酸、糖精钠(0.40 mg/kg), 脱氢乙酸(0.50 mg/kg), 纳他霉素(0.06 mg/kg); 在低(0.6~5.0 mg/kg)、中(12.5~125.0 mg/kg)、高(50.0~500.0 mg/kg) 3个加标浓度水平下, 5种目标物回收率范围为95.4%~102.8%, 相对标准偏差为0.07%~4.60%。经市售常见的半干米粉、风味香肠、果蔬汁饮料等10种食品加标测定, 回收率为92.2%~107.8%。结论 该方法适用性好、准确度高, 各项方法学指标均能符合GB/T 27404—2008《实验室质量控制规范 食品理化检测》, 可作为食品中添加剂含量测定的重要辅助手段, 以提高检验效率、提升检验质量。

英文摘要:

      Objective To establish a method for simultaneous determination of 5 kinds of additives (benzoic acid, sorbic acid, saccharin sodium, dehydroacetic acid and natamycin) content in processed foods by high performance liquid chromatography. Methods The optimal analytical conditions were determined by optimizing the gradient elution program, pH of the mobile phase, column temperature. Following the sample pretreatment procedures of national standard methods, method validation parameters (linear range, limit of quantitation, limit of detection, accuracy, precision and matrix adaptability) were evaluated using spiked recovery tests. Results The linear relationship between 5 kinds of additives was good within various concentration ranges, and the correlation coefficients (r2) were all greater than 0.999. The limits of detection (S/N=3) were determined as 0.40 mg/kg (benzoic acid, sorbic acid, saccharin sodium), 0.50 mg/kg (dehydroacetic acid) and 0.06 mg/kg (natamycin). Recoveries ranged from 95.4% to 102.8% at 3 spiked levels (low: 0.6–5.0 mg/kg; medium: 12.5–125.0 mg/kg; high: 50.0–500.0 mg/kg) with relative standard deviations of 0.07%–4.60%, with recoveries of 92.2%–107.8% in 10 kinds of commercially available foods (including semi-dry rice noodles, flavored sausages, fruit/vegetable juice beverages, etc.). Conclusion The method demonstrates high applicability and accuracy, with all validation parameters meeting the requirements of GB/T 27404—2008 Guideline on quality control of laboratories-Chemical testing of food. It can serve as a reliable supplementary approach for efficient quality control of food additives, enhancing testing efficiency and quality.