Study On The Detection Technology Of Carcinogenic Aromatic Amines And Their Salts In Textiles

The new six aromatic amines and four amine salts added to the ecological textile label OEKO-TEX（?）STANDARD 100 standard from 2019 to 2020 were studied,and new methods for detecting them were explored.The newly added aromatic amines and amine salts were analyzed together with the 24 aromatic amines involved in the original standard and applied to the detection of actual samples.By comparing the positive samples with the original detection method,this test method has better detection and recovery effect on the new aromatic amines and amine salts,and can provide technical support for daily textile detection.Twenty-eight aromatic amines and four amine salts were simultaneously determined by gas chromatography-mass spectrometry.The optimized conditions were 2 m L 40%Na OH alkalization and 10 m L tert-butyl methyl ether extraction.The linear range of 26aromatic amines was 0.05-10 mg/L,and the linear range of 2,4-diaminoanisole and2,5-diaminotoluene was 0.2-10 mg/L.The correlation coefficients were 0.996-0.999.The detection limit of 26 aromatic amines was 0.05 mg/L,and the detection limit of2,4-diaminoanisole and 2,5-diaminotoluene was 0.2 mg/L.The recoveries of2,4-diaminoanisole sulfate were 33.1%-36.0%,and the average recoveries of the other three aromatic amine salts were 84.5%-124.6%.The recoveries of 2,4-diaminoanisole were 43.7%-64.3%,and the recoveries of the remaining 27 aromatic amines were 71.7%-119.3%.Thirty aromatic amines and four amine salts were determined by liquid chromatography.The mobile phase was methanol-phosphate（potassium dihydrogen phosphate）system with methanol as the final constant volume solvent and gradient elution for 60 min.The 30 aromatic amines showed good linear relationships in the range of 0.5-10 mg/L with correlation coefficients of 0.995-0.999.The detection limits of thiazole and 26 aromatic amines were 0.1 mg/L,and the detection limits of 2,4’-diaminoanisole,p-methoxyaniline and benzidine were 0.3 mg/L.The recovery of 2,4’-diaminoanisole sulfate was 36.8%-38.3%,and the recovery of the other three aromatic amine salts was 100.4%-120.6%.The recoveries of 27 aromatic amines and 1 thiazole were 72.0-115.2%,the average recoveries of 2,4’-diaminoanisole were 63.2-65.8%,and the recoveries of 3,3-diaminobenzidine were 22.3-24.2%.A total of 224 textile samples were tested by this method.These samples contained different materials,different parts and different colors.The results of positive samples showed there was no significant difference between this method and ISO 14362 method for the detection of original aromatic amines.For newly added aromatic amines,especially 2,5-diaminotoluene,the ISO 14362 method has a risk of missed detection,and this method has a higher recovery rate.There was no significant difference between the liquid chromatography method and the gas chromatography method established in this experiment,which could be confirmed by each other and applied to the actual sample detection,providing a reference for the detection of new aromatic amines and free aromatic amine salts in OEKO-TEX^?STANDARD 100.