食品中醋磺內酯鉀、糖精、甘精及環己基（代）磺醯胺酸檢驗方法之探討及市售品調查

Developing Method for Determination of Acesulfame Potassium, Saccharin, Dulcin and Cyclamate in Process Food

檢體以水萃取，水萃取液直接經0.45 μm濾膜過濾，取濾液供作檢測醋磺內酯鉀、糖精、甘精及環己基（代）磺醯胺酸之檢液，以高效液相層析儀檢測，所使用的層析管柱為XBridge Phenyl type (5 μm, 4.6 mm i.d., ×150 mm)，以0.2%磷酸溶液與乙腈(88: 12, v/v)之混合液為分析醋磺內酯鉀、糖精及甘精之移動相溶液，以光二極體陣列檢出器，波長230 nm偵測；檢測環己基（代）磺醯胺酸時，則將檢液置於硫酸溶液中，與次氯酸鈉反應生成N, N-dichlorocyclohexylamine衍生物，以正己烷萃取，再經5%碳酸氫鈉溶液除去檢液中的游離氯後，經C18層析管柱分析，以乙腈：0.02%磷酸溶液(70: 30, v/v)之混合液為移動相溶液，以光二極體陣列檢出器，以波長314 nm偵測。研究結果顯示分離效果及重複性皆佳。蜜餞、饅頭、芋頭餡、南瓜子及冬瓜茶檢體中分別添加相當於200、100及50 ppm之醋磺內酯鉀、糖精、甘精及環己基（代）磺醯胺酸標準溶液，線性關係良好。在5種檢體中之平均回收率，分別為醋磺內酯鉀之平均回收率介於89.9~104.1%之間，且變異係數小於4.0%；糖精之平均回收率介於82.7~102.8%之間，且變異係數小於5.0%；甘精之平均回收率介於82.4~107.8%之間，且變異係數小於5.4%；環己基（代）磺醯胺酸之平均回收率介於88.1~104.8%之間，且變異係數小於3.6%。本方法醋磺內酯鉀、糖精、甘精及環己基（代）磺醯胺酸之檢出限量皆為0.001 g/kg，同日內及異日間之重複性分析變異係數分別小於5.4%及3.3%，顯示本方法之精密度可接受。

A method for the determination of acesulfame potassium, saccharin, dulcin and cyclamate in processed food by high performance liquid chromatography was developed. The samples were extracted by water, and then filtered by 0.22 μm filter. Filtrates were injected into HPLC for testing of acesulfame potassium, saccharin and dulcin on an XBridge Phenyl type (5 μm, 4.6 mm i.d., ×150 mm) column using 0.2% phosphoric acid solution: acetonitrile =88: 12 (v/v) as mobile phase. The detection wavelength was set 230 nm. The cyclamate in the sample solution was derived to N, N-dichlorocyclohexylamine with sodium hypochlorite and then extracted by hexane. The testing of N, N-dichlorocyclohexylamine was performed on a C18 (5 μm, 4.6 mm i.d., ×250 mm) column using 0.02% phosphoric acid solution: acetonitrile =30: 70 (v/v) as mobile phase. The detection wavelength was 314 nm. The results indicated that the average recoveries in five samples spiked with 50, 100 and 200 μg/mL were ranged from 89.9 to 104.1% with C. V. less than 4.0% for acesulfame potassium, from 82.7 to 102.8% with C. V. less than 5.0% for saccharin, from 82.4 to 107.8% with C. V. less than 5.4% for dulcin, from 88.1to 104.8% with C. V. less than 3.6% for cyclamate. The detection limits in five samples were all 0.001 g/kg. Their coefficients of variation of intra-day and inter-day assays were lower than 5.4% and 3.3%. These results indicated that the developed method was satisfactory.