高效液相色谱法测定甜菊糖甙中的甜蜜素

Determination of cyclamate in stevioside by high performance liquid chromatography

目的：建立高效液相色谱法测定食品添加剂甜菊糖甙中甜蜜素的检测方法。方法样品,经水溶解后无需添加沉淀剂,加入衍生试剂,最后采用高效液相色谱法进行测定。对称样量、流动相的选择、沉淀剂的使用和衍生化试剂的用量进行研究,确定0.5 g称样量,4 mL衍生试剂次氯酸钠溶液衍生10 min,加入25 mL 50 g/L NaHCO3溶液,振荡萃取。结果甜蜜素浓度在2.5~25.0 mg/kg的范围与峰面积成线性关系,线性相关系数为0.9991,甜蜜素的回收率为81.8%~95.0%之间、RSD(n=6)为1.21%~2.07%,方法检测限为2.5 mg/kg。结论该方法操作简便,准确可靠,可用于鉴别甜菊糖甙中掺入的甜蜜素。

ABSTRACT:Objective To establish a method for the determination of cyclamate by high performance liq-uid chromatography. Methods These factors including mobile phase, pH and derivatization time, and the amount of derivatization reagent were investigated. The samples were derivatived after being dissolved directly without precipitating agent, the amount of derivatization reagent was 4 mL, and the derivating time was 10 min. Methanol+water (75+25, v/v) was selected as the eluent. Results The linear relationships between the con-centration and peak area were obtained in the concentration range of 2.5～25.0 mg/L with R2=0.9991. The reco-veries were 81.8%~95.0%with the relative standard deviations (n=6) of 1.21%~2.07%, and the detection limit was 2.5 mg/kg. Conclusion The method is simple, accurate and reliable.