高效液相色谱-二极管阵列检测器同时测定糕点中糖精钠和脱氢乙酸的方法研究

Investigation on the measurement of saccharin sodium and dehydroacetic acid in cookies by HPLC coupled with photo-diode array detector

建立了糕点中糖精钠和脱氢乙酸同时测定的高效液相色谱法。糕点样品经氢氧化钠、硫酸锌沉淀后,以甲醇-10mmol/L醋酸铵(PH=5.5)为流动相,梯度洗脱,经AtlantisT3C18色谱柱分离,二极管阵列检测器检测,外标法定量。结果表明:在0.4~50μg/mL浓度范围内,两种物质线性关系良好,线性相关系数均大于0.9999。在5mg/kg、10mg/kg、50mg/kg三个浓度加标水平下,糖精钠和脱氢乙酸的回收率分别为85.0%~101.2%和87.3%~97.9%,相对标准偏差均小于10%。该方法操作简单、快速、准确,能满足复杂糕点基质中两种化合物同时测定的要求。

A HPLC(high performance liquid chromatographic)method was developed to simultaneously analyze saccharin sodium and dehydroacetic acid in cookies.The pastry samples were treated by 1mL 0.5mol/L zinc sulfate solution and 1mL 1.0mol/L sodium hydroxide solution.The sample solutions were separated on an Atlantis T3 C18 column using methanol-10mmol/L ammonium acetate(PH=5.5)as the mobile phase in gradient elution mode.The quantitation was achieved by the photo-diode array detector with the external standard method.The results showed that both of the two compounds had good linear relationships in the concentration range of 0.4~50μg/mL,and the linear correlation coefficients were greater than 0.9999.The recoveries of saccharin sodium and dehydroacetic acid were 85.0%~101.2%and 87.3%~97.9%at the levels of 5 mg/kg,10 mg/kg and 50 mg/kg of standard substance,respectively.The relative standard deviations were less than 10%.The method is simple,rapid and accurate,and can meet the requirements of simultaneous determination of saccharin sodium and dehydroacetic acid in pastry samples.