食品科学 ›› 2008, Vol. 29 ›› Issue (12): 507-510.

• 分析检测 • 上一篇    下一篇

Carrez试剂沉淀-气相色谱法测定复杂基质食品月饼中的甜蜜素

 应兴华, 徐霞, 陈能, 翟远建, 朱敏   

  1. 中国水稻研究所农业部稻米及制品质量监督检验测试中心; 中国计量学院;
  • 出版日期:2008-12-15 发布日期:2011-12-08

Determination of Sodium Cyclamate in Moon Cake Matrix by Using Gas Chromatography after Precipitation with Carrez Reagent

 YING  Xing-Hua, XU  Xia, CHEN  Neng, DI  Yuan-Jian, ZHU  Min   

  1. 1.Rice Product Quality Supervision and Inspection Center,Ministry of Agriculture,China National Rice Research Institute, Hangzhou 310006,China;2.China Jiliang University,Hangzhou 310018,China
  • Online:2008-12-15 Published:2011-12-08

摘要: 建立了应用Carrez试剂沉淀、亚硝酸酯化和气相色谱、氢火焰离子化检测器测定复杂基质食品月饼中甜蜜素的方法。考察了不同提取方式(高速匀浆、超声和研磨)的提取效率和Carrez试剂用量对甜蜜素测定的影响。试样经高速匀浆提取、Carrez试剂沉淀分离杂质后,在硫酸介质中经亚硝酸酯化,衍生物经气相色谱分离、氢火焰离子化检测器测定。方法的检出限为2mg/kg(S/N=3)。在添标水平为0.25、0.50和1.0mg/g时的平均添加回收率为85.12%~99.38%,相对标准偏差6.44%~8.31%。衍生物的峰面积与样品浓度在0.125~1.0g/L范围内呈良好的线性关系,相关系数为0.9992。该方法仪器设备简单,测定结果准确、可靠,适合复杂基质食品中甜蜜素的测定。

关键词: 气相色谱, 复杂基质, 月饼, 甜蜜素, 样品前处理

Abstract: An analytical method of gas chromatography with flame ionization detection after precipitation with Carrez reagent was developed and validated for determination of sodium cyclamate in moon cake matrix. The effects of Carrez reagent amount on determination of sodium cyclamate and the extraction efficiencies of homogenization,ultrasonic and grinding methods were extensively investigated. After homogenization,samples were cleaned-up with Carrez reagent and derived with nitrite sodium and sulphuric acid,and the cyclohexyl nitrite was analyzed by using gas chromatography with flame ionizator detector. At 0.25,0.5 and 1.0 mg/g fortification levels,the average recoveries range from 85.12% to 99.38% with the relative standard deviations from 6.44% to 8.31%. The method shows good linearity over the range assayed 0.125 to 1.0 g/L and the detection limit is 2 mg/kg. It is suitable for determination of sodium cyclamate in complex matrix food with rapidity,sensitivity and accuracy.

Key words: gas chromatography, complex matrix, moon cake, sodium cyclamate, sample preparation