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衍生HPLC法快速检测食品中微量甜蜜素含量

Rapid determination of micro sodium cyclamate in food by HPLC with derivatization

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【作者】 王坤唐洪年娟

【Author】 WANG Kun,TANG Hong,NIAN Juan(Yancheng Center for Disease Control and Prevention,Yancheng 224002,China)

【机构】 江苏省盐城市疾病预防控制中心

【摘要】 目的:建立衍生HPLC法快速检测食品中微量甜蜜素的方法。方法:甜蜜素本身无紫外吸收,利用环己基胺基磺酸钠与次氯酸钠在酸性环境中衍生反应,生成N,N-二氯环己胺,再被正己烷萃取出来,在XDB-C18柱上,以甲醇(V):水(V)=80:20为流动相进行分离,检测波长314 nm,外标法定量。结果:建立了快速、有效的分离和样品处理方法。甜蜜素的浓度在0~300μg/ml之间呈线性关系,相关系数0.9995以上,且准确度、重现性好。回收率为85.3%~97.5%,RSD为2.32%~6.36%之间,方法最低检出限为0.5 mg/kg。结论:该方法快速简便,灵敏度高,干扰少,适用于大部分食品样品的测定。

【Abstract】 Objective:To develop a method for the determination of micro sodium cyclamate in food by high performance liquid chromatography(HPLC) with derivatization.Methods:Traditional HPLC is not suitable for the determination of cyclamate because cyclamate itself does not absorb in ultraviolet/visible(UV/VIS) region.But N,N-dichloridecyclohexane can be detected,which is produced by the reaction between cyclamate and hypochlorous sodium.N,N-dichloridecyclohexane was extracted into n-hexane from the solution and was separated on XDB-C18 column by using a mobile phase of methanol(V): water(V)=80:20,then detected by ultraviolet/visible(UV/VIS) monitor at 314nm.External standard method was used for quantification.Results:An improved technique for the rapid detection,effective separation and sample processing was established.The linear range of sodium cyclamate was 0~300 μg/ml with linear correlation coefficient of 0.9995.The result is reproducible and accurate.The recovery of the method for sodium cyclamate is 85.3%~97.5%,the coefficient of variation is 2.32%~6.36% and the limits of quantification is 0.5 mg/kg.Conclusion:This method is simple,rapid,sensitive and of little interference.It can be successfully applied to the measurement of cyclamate in food.

  • 【文献出处】 中国卫生检验杂志 ,Chinese Journal of Health Laboratory Technology , 编辑部邮箱 ,2009年12期
  • 【分类号】TS207.3
  • 【被引频次】2
  • 【下载频次】109
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