Central Science Laboratory, Sand Hutton, York, UK.
Food Addit Contam Part A Chem Anal Control Expo Risk Assess. 2009 May;26(5):614-22. doi: 10.1080/02652030802695480.
A method for the determination of cyclamate has been developed and single-laboratory validated for a range of foodstuffs including carbonated and fruit-juice drinks, fruit preserves, spreads, and dairy desserts. The method uses the peroxide oxidation of cyclamate to cyclohexylamine followed by derivatization with trinitrobenzenesulfonic acid and analysis by a modified reversed-phase high-performance liquid chromatography-ultraviolet light (HPLC-UV). Cycloheptylamine is used as an internal standard. The limits of detection were in the range 1-20 mg kg(-1) and the analysis was linear up to 1300 mg kg(-1) cyclamic acid in foods and up to 67 mg l(-1) in beverages. Analytical recovery was between 82% and 123%, and results were recovery corrected. Precision was within experimentally predicted levels for all of the matrices tested and Horrat values for the combined standard uncertainty associated with the measurement of cyclamate between 0.4 (water-based drinks) and 1.7 (spreads). The method was used successfully to test three soft drink samples for homogeneity before analytical performance assessment. The method is recommended for use in monitoring compliance and for formal testing by collaborative trial.
已开发出一种环氨酸盐的测定方法，并对一系列食品（包括碳酸饮料和果汁饮料、水果蜜饯、涂抹酱和乳制品甜点）进行了单实验室验证。该方法使用环氨酸盐的过氧化物氧化生成环己基胺，然后用三硝基苯磺酸衍生化，并用改良的反相高效液相色谱-紫外光（HPLC-UV）进行分析。环己基胺用作内标。检测限范围为 1-20mgkg(-1)，在食品中环氨酸酸的分析线性范围为 1300mgkg(-1)，在饮料中可达 67mg l(-1)。分析回收率在 82%至 123%之间，并进行了回收率校正。对于所有测试的基质，精密度均在实验预测范围内，并且与环氨酸盐测量相关的组合标准不确定度的 Horrat 值在 0.4（基于水的饮料）和 1.7（涂抹酱）之间。该方法成功地用于在分析性能评估之前测试三种软饮料样品的均一性。该方法推荐用于监测法规遵从性和协作试验的正式测试。
