Method Study And Application On The Determination Of Food Additives In Food By Chromatography

Objective:In this paper,a serials of chromatography methods were established to test 11 kinds of food additives in food rapidly, with which ,a survey was made to estimate the sanitary safety of retail food in Jinan city.Methods:1. Additives to be tested: Saccharin, Sodium cyclamate, Acesulfame potassium, benzoic acid, sorbic acid, Sulphites, Tartrazine, Sunset yellow, Amaranth, Ponceau 4R, Brilliant blue.2. Analytical methods2.1 Clear liquid products were diluted with water and fiiltered through a membrane filter of pore size 0.45 urn. Load sample solutions to determinate 9 kinds of food additives onto column and use gradient elution to achieve optimum separation with the mobile phase consisted of methanol -0.02 mol/L ammonium acetate,then detected by diode array detector .Technical parameters of the method were optimized and confirmed,including gradient profile, detection wavelength ,nearity,LODs,RSD, recovery rate and comparetive test.2.2 Samples with complex matrix were extracted with water by ultrasonic cleaner and purified with potassium ferrocyanide solution and zinc acetate solution. Then sample solutions to determinate 4 kinds of food additives were performed on Kromasil C18 column and detected by diode array detector, with the mobile phase consisted of methanol -0.02 mol/L ammonium acetate(6:94, V/V). Technical parameters of the method were optimized and confirmed.2.3 Samples with complex matrix were extracted with alcohol-ammonia-water solution and purified with polyamide. Then sample solutions were performed by HPLC with gradient elution . In the research,technical parameters of the method were optimized and confirmed.2.4 Samples were distilled and absorbed by H₂O₂ aqueous.Then sample solutions to determinate sulfate were performed on AS18 anion column and detected by ECD, with KOH solution as the mobile phase. The method were optimized and confirmed,including chromatography parameters,distillation conditions,etc. 2.5 Sodium cyclamate was determinated with standard method in law.3. Survey in Jinan: Some kinds of food,such as grape wine, biscuit, were collected from different sales terminal,including super markets,marketplaces,etc.Then these samples were determinted with methods mentioned in the paper,to learn the sanitary safety of retail food in Jinan city.Results:1. Food additives mentioned in the paper were separated thoroughly with definied conditions. Correlation coefficient of calibrations were between 0.9996-1.0000.Range of RSD 1.03%-6.10%; Range of recovery rate 85.5-103.0%.2. In the survey,of the 328 samples, food additives mentioned in the paper could be tested in 278 samples and the concentrations over the permitted limits were in 73 samples. The detected ratio and overlimit ratio were 84.76%,22.26%.Conclusions:1. With accuracy,reproducibility and good linearity,as long as convenient sample preparations,these methods in the paper were feasible to detect food additives in routine work and market survey2. The detected ratio and overlimit ratio of 11 kinds of food additives were quite high in retail food in Jinan city,especially in preserved fruits, moon cakes,etc.The sanitary situation of these foods were good relatively that were sold in super market or produced by powerful enterprise.