Study On Detection Methods Of 11 Kinds Of Illegally Added Industrial Dyes In Bean Products

Industrial dyes are carcinogenic,teratogenic and mutagenic to human body,in recent years,the illegal addition of industrial dyes in food occurs frequently,which seriously harms the health of consumers.Eleven industrial dyes(Dimethyl Yellow,Diethyl Yellow,Auramine O,Solvent Yellow 124,Sudan Orange G,Basic Orange 2,Basic Orange 21,Basic Orange 22,Metanil Yellow,Acid Orange?,Orange?)which may be illegally added to bean products were selected,solid phase extraction-high performance liquid chromatography and ultra high performance liquid chromatography-tandem mass spectrometry were established.The research includes:1.A solid phase extraction method was developed for the simultaneous determination of 11illegal industrial dyes in soybean products by using solid phase extraction(SPE-HPLC).Select0.05mol/L ammonium acetate solution+methanol+formic acid(V/V/V=50/49/1)as the extraction solvent to extract the sample,Strata-x-aw solid phase extraction column was used for purification,ammonia water was eluted with methanol,and tested by 0.22?m PTFE membrane.The Water Symmetry C₁₈column was used for separation,the detection wavelength was450nm,The mobile phase was methanol-0.02mol/L ammonium acetate solution.Under the optimized chromatographic conditions,11 kinds of illegally added industrial dyes have good linearity in the concentration range of 0.5?100 mg/L.The correlation coefficient(R²)was greater than 0.9956.The recovery of standard addition of soybean products is 75.0%?95.0%,and the relative standard deviation is 1.6%?5.0%.The detection limit of Solvent Yellow 124 is 0.16mg/kg,the quantitative limit is 0.54 mg/kg,the detection limit of other 10 industrial dyes is 0.02mg/kg,the quantitative limit is 0.06 mg/kg.2.A method was developed for the determination of 11 illegal industrial dyes in soybean products by ultra High-performance liquid chromatography tandem mass spectrometry(UPLC-MS/MS).After the bean products are evenly stirred,they are extracted by acidification of acetonitrile aqueous solution,the supernatant is added with sodium chloride for salting out and layering,frozen at-20?for 2h,and centrifuged at high speed,which could effectively remove the protein interferences in soybean products.After filtration in acetonitrile layer and gradient elution,it was separated by Hypersil Gold Dim column and detected by multi ion reaction monitoring mode(MRM),Three kinds of industrial dyes(Metanil Yellow,Acid Orange?,Orange?)use the negative ion mode,acetonitrile–0.01 mol/L ammonium acetate solution as the mobile phase,the other eight kinds of industrial dyes use the positive ion mode,and 0.1%acetonitrile formate solution-0.1%formic acid aqueous solution as the mobile phase.The correlation coefficients(R²)of 11 industrial dyes were higher than 0.9918.The recovery of standard addition was 73.3%-90.0%,the relative standard deviation was 1.4%-6.5%,the detection limit was 0.1-1.8?g/kg,and the quantitative limit was 0.3-5.3?g/kg.3.The two methods can be used for the detection of 11 kinds of orange industrial dyes illegally added to bean products.40 samples of bean products(10 dried beancurd,10 dried beancurd,10 plain chicken and 10 dried beancurd skin)from the surrounding markets and supermarkets were analyzed by two methods.The results showed that the same beancurd sample contained There was alkaline yellowish o,and the content was similar.The experimental results show that the two detection methods can not only be used as an independent method to detect the illegal addition of industrial dyes,but also complement and contrast the analysis and determination of the illegal addition of industrial dyes in bean products.In general,SPE-HPLC has good repeatability,accurate quantification and low hardware requirements.Ultra high performance liquid chromatography tandem mass spectrometry(UPLC-MS/MS)is characterized by high accuracy,low detection limit,short analysis time and wide analysis range.