柿饼中10种禁用食品添加剂的高效液相色谱分析方法研究

Study on the determination of 10 illegal food additives in dried persimmon by high performance liquid chromatography method

建立了一种同时测定柿饼中安赛蜜、苯甲酸、山梨酸、糖精钠、柠檬黄、新红、苋菜红、胭脂红、日落黄、诱惑红的高效液相色谱分析方法。对提取试剂、流动相条件、检测波长进行了研究,确定了最佳提取方法及色谱条件。样品经70%乙醇水（v/v）超声波提取,以C18（250mm×4.6mm,5μm）为分析柱,甲醇和乙酸铵溶液为流动相进行梯度洗脱,可变波长程序进行检测,流速为1m L/min,以色谱峰保留时间和紫外可见光谱进行定性,外标法进行定量。10种添加剂分别在0.01~0.05mg/m L、0.001~0.005mg/m L范围内线性关系良好（R2〉0.999）,方法检出限为0.03~0.15mg/kg。在低中高3个标样添加水平（100、200、300mg/kg,5、10、25mg/kg）下10种添加剂的回收率在85%~94%,相对标准偏差（n=6）为1.2%~2.6%。该方法简单、快速、灵敏、准确,适用于柿饼中添加剂的检测分析。

A high performance liquid chromatography method was established for the simultaneous determination of 10 illegal food additives including acesulfame potassium,benzoic acid,sorbic acid,sodium saccharin,tartrazine,new red,amaranth,ponceau 4R,sunset yellow and allura red in dried persimmon. The optimal extraction conditions and HPLC chromatographic conditions were confirmed by investigating the extracting solvent,mobile phase type and absorption wavelength. The samples was extracted by ultrasonic with 70%（v/v） ethanol water. The separation was performed on an C18 column using a mobile phase consisting of carbinol and acetic ammonium solution mixture by gradient elution and variable wavelength detection at a flow rate of 1.0m L/min.The retention time and UV visible spectroscopy was used in qualitative analysis and the external standard method was used in quantitative analysis. The calibration curves of 10 additives showed good linearity（R2 0.999）in the range respectively of 0.01 ~ 0.05mg/m L and 0.001 ~ 0.005mg/m L. The detection limits were in the range of 0.03 ~ 0.15mg/kg. The recoveries ranged from 85% ~ 94% at 3 spiked levels（100,200,300mg/kg and 5,10,25mg/kg）with RSDs（n=6）of 1.2% ~ 2.6%. The method was simple,rapid,sensitive and accurate,and was suitable for the determination of food additives in dried persimmon.