高效液相色谱法测定饮料中防腐剂和甜味剂

HPLC Determination of Saccharine Sodium,Benzoic Acid,Sorbic Acid and Sodium Cyclamate in Carbonic Drink

建立了高效液相色谱-示差折光检测器法同时测定碳酸饮料中苯甲酸、山梨酸、糖精钠、甜蜜素的分析方法,考察了流动相配比、缓冲溶液的浓度、柱温、检测器的温度及灵敏度设置对测定的影响,确定了最佳色谱条件:Novopak-C18柱,示差折光检测器(RID),流动相为甲醇-0.010mol/L乙酸铵溶液(3:97,V/V),等度洗脱方式,柱温及RID检测器温度30℃,RID检测器灵敏度设置64。结果显示,线性范围为2.0～200μg/ml,相关系数为0.9995～0.9999,检出限依次为0.2、0.2、0.2、1.3μg/ml,相对标准偏差2.1%～3.5%,平均回收率89.0%～104.5%,实现了7min内对碳酸饮料中苯甲酸、山梨酸、糖精钠、甜蜜素的同时测定。

A high-performance liquid chromatographic method was described for the simultaneous determination of saccharine benzoic acid, sorbic acid sodium, and sodium cyclamate in carbonic drink. The effects of operation conditions of HPLC such as the component of the mobile phase, the concentration of ammonium acetate, column and detector temperature, and detector sensitivity setting on determination were investigated. The optimal conditions are as follows： reversed-phase Novo pak-C18 column used for separation with refractive index detector（RID） for detection. Methanol-ammonium acetate （3：97, V/V） as the mobile phase with isocratic elution, column temperature 30 ℃. RID detector sensitivity 64. Under the best conditions, the calibration curve is linear between 2.0μg/mland 200.0 μg/ml. The correlation coefficients ranges from 0.9995 to 0.9999. The detection limits are 0.2, 0.2, 0.2, 1.3la g/rnl respectively. The recoveries of four compositions are 89.0%~ 104.5%. The relative standard deviations （RSD） are in the range from 2.1% to 3.5%.