Acetylsulfonamide potassium (Acesulfame) detection

Preparation method 1: Acetylacetamide, sulfur trioxide, and KOH are used as raw materials. Firstly, acetylacetaminosulfonic acid is synthesized in an inert organic inorganic solvent, and SO3 is introduced into acetylacetamide for cyclic condensation. Then extract and separate it, and then react with KOH to obtain the product. For example, at -60 ℃, 5.1g (50mmol) of acetylacetamide dissolved in 50mL of CH2Cl2 is dropwise added to 8mL (200mmol) of liquid SO3 dissolved in 50mL of CH2Cl2. After stirring for 2 hours, 50mL of ethyl acetate and 50mL of water are added to the solution. After extraction, the organic phase is separated. Extract the aqueous phase twice with ethyl acetate, and merge the resulting organic liquid into the organic phase. Dry on anhydrous Na2SO4 and evaporate to recover ethyl acetate. The remaining substance is dissolved in methanol and neutralized with KOH solution to precipitate acesulfame. After drying, 3.1g of the product is obtained with a recovery rate of 31% of the theoretical amount. The disadvantage of this method is that the reaction needs to be carried out at a relatively low temperature and the yield is not high&Nbsp; 2. Add 9.7g (0.1mol) of aminosulfonic acid to 16mL (0.12mol) of triethylamine using aminosulfonic acid, triethylamine, dienone, SO3, and KOH as raw materials. Stir until completely dissolved, then add 8mL of dienone dropwise at 0 ° C and stir at room temperature until the reaction is complete. Add hexane to precipitate and refine. Under reduced pressure, the solvent is removed to obtain a slurry with a yield ranging from 95.7% to 99.0%. At -30 ℃, add the slurry with 5-6 equivalents to a container containing CH2Cl2 and stir continuously for 1-5 hours. Depressurize the solvent, treat the remaining KOH solution at pH=8-10, and remove the solvent and dry to obtain acesulfame in a yield of 69%. The advantage of this method is that the raw materials are easily available, the process conditions are relatively mild, but the process is complex&Nbsp; 3. Using aminosulfonyl fluoride, diene ketone, potassium carbonate, and KOH as raw materials at 0 ℃, the diene ketone is dropwise added to an acetone solution of H2NSO2F and K2CO3 to obtain a potassium salt of ethylphenolhexylamino-N-sulfophthalide fluoride. It reacts with CH3OH and KOH solutions to obtain acesulfame. For example, dissolve 76g (0.55mol) of K2CO3 powder in 500mL of acetone, add 57.8mL (1.0mol) of H2NSO2F, dropwise add 84.3mL (1.1mol) of dienone within 15 minutes, stir and mix at 0 ℃ for 30 minutes, and an exothermic reaction occurs. Control the temperature below 30 ℃ until CO2 is completely released, and the reaction can be stopped. Filter the reaction mixture and wash with a small amount of acetone. To obtain a colorless crystalline potassium salt of acetylacetamido-N-sulfonphthalide fluoride. Stir this potassium salt with a 4-6mol methanol solution to cyclize into acesulfame. The yield is 93% of the theoretical amount. [3] Application field: As a non nutritive sweetener, the concentration of acesulfame in food and beverages remains basically unchanged within the general pH range. It can be mixed with other sweeteners, especially when combined with aspartame and cyclohexylaminosulfonate for better results. It can be widely used in solid drinks, Pickled vegetables, candied fruits, gums, table sweeteners and other foods. This product has a strong sweet taste, with a sweetness about 200 times that of sucrose. Its taste properties are similar to those of saccharin, and it has a bitter taste at high concentrations. According to the National Food Safety Standard for the Use of Food Additives (GB 2760-90) in China, the maximum usage amount is 0.3g/kg. It can be used as a sweetener in food, medicine, and other fields. The regulations and standards of international organizations, countries, and regions such as the Codex Alimentarius Commission (CAC), the European Union, the United States, Japan, Australia, New Zealand, and Canada allow acesulfame to be used as a sweetener in corresponding foods. In some European and American countries, acesulfame can be used in sweet products. [1] According to the "National Food Safety Standards for the Use of Food Additives" (GB 2760-2014) in China, acesulfame can be used in ready-to-eat flavored foods with milk as the main ingredient or its prefabricated products (excluding ice cream and flavored fermented milk) (limited to canned milk based desserts), frozen beverages (excluding edible ice), canned fruits, jams, preserves, pickled vegetables, processed edible mushrooms and algae, canned grains, black sesame paste Canned cereal desserts, baked goods, beverages (excluding packaged drinking water), jellies, table sweeteners, seasonings, soy sauce, candies, gum based candies, etc., but are not allowed to be used in cold fruit products. China has also formulated corresponding quality specification requirements for Acesulfame, namely "National Food Safety Standard for Food Additive Potassium Acetosulfonate" (GB 25540-2010). In addition, according to the General Principles for the Labeling of Prepackaged Food in accordance with the National Food Safety Standards (GB 7718), as long as acesulfame (including the use of compound sweeteners containing acesulfame) is used in food, it must be labeled on the food label&Nbsp

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