高效液相色谱法测定保健饮品中的环己基氨基磺酸钠  

The determination of sodium cyclamate in health beverage by high performance liquid chromatography

作　　者：董曼曼 卫星华 张凡 孙晓 王涛 DONG Man-Man;WEI Xing-Hua;ZHANG Fan;SUN Xiao;WANG Tao(Xi'an Institute for Food and Drug Control,Xi'an 710054)

机构地区：[1]西安市食品药品检验所

出　　处：《中国食品添加剂》2019年第7期192-197,共6页China Food Additives

基　　金：陕西省科技厅科技统筹创新工程计划项目（2014FWPT-01）;陕西省科技厅重点研发计划（2017F-311）;陕西省科技研究发展计划项目（2013K13-04-06）;西安市碑林区科技局应用技术研发项目（GX1706）

摘　　要：目的:优化高效液相色谱(HPLC)测定保健饮品中环己基氨基磺酸钠(甜蜜素)含量的方法。方法:环己基氨基磺酸钠用水提取后,在强酸性溶液中与次氯酸钠反应,生成N,N-二氯环己胺,用正己烷萃取后,利用高效液相色谱法检测。结果:甜蜜素含量在9.09~910mg/kg范围内峰面积与甜蜜素含量呈良好的线性关系,加标回收率在97.9%~101%之间。用正己烷作为提取溶剂时,普通液体和含乳保健饮品的回收率分别为101%和97.5%,而用正庚烷作为提取溶剂时,回收率分别为94.1%和88.4%;衍生试剂加入顺序为次氯酸钠、正己烷、硫酸时,回收率为103%,结果最好;衍生产物在室温下16h内稳定性较好;含乳保健饮料不除蛋白时回收率更高,为101%。结论:用正己烷作为提取溶剂,衍生试剂加入顺序为次氯酸钠、正己烷、硫酸,含乳保健饮料不除蛋白时回收率更高、精密度更好。本实验优化后的方法可为检测保健饮品中的甜蜜素提供一定参考。Objective : The HPLC method for the determination of sodium cyclamate in health beverage was optimized. Methods : Firstly, the sodium cyclamate was extracted by water, and then it reacted with sodium hypochlorite in strong acid solution to generate N, N-dichlorocyclohexylamine. After extraction with n-hexane, HPLC was used for the determination. Results : The results showed that the linear relationship was good within the range from 9.09 to 910mg/kg between values of peak and mass concentration of sodium cyclamate, with the recoveries ranged 97.9%~ 101%. When n-hexane was used as the extraction solvent, the recovery of ordinary liquid and dairy health beverage were 101% and 97.5% respectively, while when n-heptane was used as the extraction solvent, the recovery were 94.1% and 88.4% respectively. When the order of adding derivative reagents was sodium hypochlorite, hexane and sulfuric acid, the recovery was 103% and the result was the best. The derivative was stable at room temperature for 16h and the recovery rate of dairy health beverage was 101% without protein removal. Conclusion : When the extraction solvent isn-hexane and the order of adding derivative reagents is sodium hypochlorite, n-hexane and sulfuric acid and the dairy health beverage without protein removal, the recovery was higher and the precision was better. The method optimized in this study can provide reference for the determination of cyclamate in health beverage.

关 键 词：高效液相色谱法 甜蜜素 保健饮品 提取溶剂 衍生试剂 

分 类 号：TS202.3[轻工技术与工程—食品科学] O657.72[轻工技术与工程—食品科学与工程]