Research on Analysis Methods for Sodium Cyclamate, Sodium Saccharim, Benzoic Acid, Sobic Acid in Food
|Keywords||Cyclamate Sodium Saccharin Benzoic acid Sorbic acid High Performance Liquid Chromatography Differential refractive index detector UV spectrophotometry|
In order to improve the quality of food and color, smell and taste as well as the preservation or processing needs, usually in food sodium cyclamate, sodium saccharin, benzoic acid and sorbic acid, these substances excessive use of hazard to human health. National Institute of Standards determination of sodium saccharin and benzoic acid and sorbic acid using high performance liquid chromatography - UV detector was measured samples without derivatives, can be directly measured, sodium cyclamate no absorption in the ultraviolet region, need to derivative by gas chromatography or high-efficiency simultaneous determination of liquid chromatography determination alone, tedious step, increased costs, while limiting sodium cyclamate and other sweeteners and preservatives, rather than derived directly using high performance liquid chromatography for the determination of cyclamate, saccharin in food , sodium benzoate and sorbic acid have not been reported for high performance liquid chromatography instruments used in higher prices at the same time, is not suitable for small laboratory to detect the need for a separate cyclamate, to establish simultaneous determination of cyclamate, benzoic acid , sorbic acid and saccharin sodium, high performance liquid chromatography method and universal, easy and accurate, suitable for medium and small laboratory rapid determination of sodium cyclamate is very necessary. In this thesis, using high performance liquid chromatography - a differential detector analysis method for the simultaneous determination of sodium cyclamate in food, sodium saccharin, benzoic acid and sorbic acid. The effects of mobile phase system, the ratio of the concentration of ammonium acetate solution, including flow rate, column temperature, the temperature of the detector and sensitivity settings, the injection volume was measured to determine the best chromatographic conditions: column Novo-pak C18 column; differential refractive index detector; mobile phase methanol: ammonium acetate (0.01mol / L) = 3:97 (V: V); the detected temperature 30 ° C, a differential refractive index detector sensitivity setting 64; column temperature 30 ° C; flow rate of 1.0ml/min; the injection volume 10.0μL. In optimum conditions, the establishment of the four components of the linear regression equation, correlation coefficient of 0.9995-0.9999, the linear range 0.7-200μg/mL. The minimum detectable concentration was 0.2-1.3μg/mL sample minimum detectable amount of sodium cyclamate 6.5μg / g, sodium saccharin 1.0 ug / g benzoic acid 1.0 ug / g, sorbic acid is 1.0 ug / g The average recovery of 89.0% -114.5% and the relative standard deviation of 2.1% -3.5% within 7 min determination of sodium cyclamate, sodium saccharin, benzoic acid and sorbic acid, while this method is used in real samples square analysis with satisfactory results. Indirect UV spectrophotometric determination of cyclamate in food. ScS acidic medium, sodium nitrite, potassium iodide concentration, dosage and reaction time as well as reagents joined sequentially measured to obtain the optimum conditions for the 2.5 mol / LHCl 1.0 mL, 2.0 mmol / L sodium nitrite in 1.6 mL reaction measured after 10 min, 0.05mol / L KI solution 2.0 mL, dark place for 10 min. In optimum conditions, sodium cyclamate obeys Beer's law in the range of 1.0-14.0μg/mL the linear equation A = 0.5702c 0.0006, r = 0.9984, the minimum detectable concentration was 0.3μg/mL minimum sample detectable amount of 7.5μg / g, the average recovery was 102.3% -103.3% and the relative standard deviation of 0.7% -1.3%. This method is experimental, low cost, universal, suitable for routine laboratory rapid determination of sodium cyclamate in food.