飲料中醋磺內酯鉀、糖精、阿斯巴甜、甜精及環己基代磺醯胺酸之檢驗方法探討及含量調查

Determination of Acesulfame K, Saccharin, Aspartame, Dulcin and Cyclamate in Beverages

本研究探討以高效液相層析法（HPLC）同時檢測飲料中醋磺內酯鉀（acesulfame K）、糖精（saccharin）、阿斯巴甜（aspartame） 及甜精（dulcin）四種人工甘味劑之方法。對於無法由紫外光檢出器檢測之環己基代磺醯胺酸（cyclamate），則以高效離子層析法（HPIC）進行分析。HPLC方法乃是檢液先經ODS-4淨濾器淨化後，使用Bondapak C18 （3.9×300mm, 10µm）層析管，以磷酸調成pH值6 之34mM TEA-OH 及甲醇（80:20 , v/v）溶液為移動相，於流速1mL/min，UV 210 nm 波長條件下，歷時30分鐘可同時檢出acesulfame K、saccharin、aspartame及dulcin。添加適量混合標準溶液於碳酸飲料類、乳酸醱酵飲料類、運動飲料類、果汁類及茶湯類中，使其最終濃度為各含四種人工甘味劑100ppm及200ppm之檢液，則acesulfame K、saccharin、aspartame及dulcin回收率可達92.2%以上。對於cyclamate分析，則另以AS4A-SC 及AG4A-SC離子層析分析管和保護管，經5mM Na2B4O7，為溶離液，於流速1.85mL/min，電傳導檢出器在輸出範圍為10μS條件下，進行HPIC分析。添加適量之cyclamate標準溶液於上述五類飲料中，使其最終濃度為含cyclamate 100ppm及200ppm之檢液，則其回收率可達92.7%以上。五十件市售飲料中標示含有一種人工甘味劑者計有五件，含有兩種人工甘味劑者計有兩件（cyclamate & saccharin、acesulfame K & aspartame）。檢測結果，除一件標示含cyclamate者（含量為894ppm）遠超過我國衛生限量標準200ppm之外，另有標示含acesulfame K者計一件（含量為100ppm），標示合saccharin者計一件（含量為100ppm），標示含aspartame者共計七件（含量在35～560ppm），其餘則未檢出含人工甘味劑。

Four artificial sweeteners, i.e. acesulfame K, saccharin, aspartame and dulcin, in beverages were determined simultaneously by high performance liquid chromatography (HPLC) whereas cyclamate was analyzed by high performance ion chromatography (HPIC). These four sweeteners, adsorbed by ODS-4 cartridges then eluted with the mixture of methanol and phosphate buffer, were analyzed in a reversed phase mode with ion-pair reagent and detected by UV absorption at 210 nm. Cyclamate, with poor UV absorption, was analyzed by Dionex AS4A-SC column eluted with 5 mM Na2B4O7 solution and detected by a conductivity detector. Recoveries of acesulfame K, saccharin, aspartame and dulcin fortified at 100 ppm and 200 ppm levels in beverages, including carbonated drinks, sport drinks, lactic acid milk drinks, juice and tea extract, were above 92.2%. Recoveries of cyclamate spiked into beverages at 100 ppm and 200 ppm fortification levels were above 92.7%. Fifty samples collected from supermarkets were analyzed. The results showed, a sample labelled cyclamate contained 894 ppm which was highly over the hygienic limitation of 200 ppm. One of saccharin, one of acesulfame K and seven of aspartames were also labelled and matched the detections, which were 100 ppm, 100 ppm and between 35-560 ppm, respectively. They were all below the limitation. The others were not labelled and the sweeterners mentioned aboved were non detectable.