高效液相色谱荧光法测定全棉织物中微量苯胺和二苯胺

Determination of trace aniline and diphenylamine in cotton fabric using high performance liquid chromatography with fluorescence detection

建立了全棉织物中苯胺、二苯胺的高效液相色谱荧光分析方法。全棉织物采用乙腈/甲苯（3/1,V/V）为提取剂,以Carb/PSA固相萃取小柱进行净化,在Kromasil C18柱（250 mm×4.6 mm i.d.,5μm）上以水/乙腈（25/75,V/V）为流动相进行分离,采用荧光法进行检测,荧光检测波长λex为280 nm,λem为340 nm。结果表明,苯胺、二苯胺的低、中、高3个加标水平下的平均回收率分别为97.3%-103.5%和98.0%-103.4%,相对标准偏差分别为1.4%-4.2%和0.98%-4.7%,方法的检出限分别为0.3μg/kg和0.2μg/kg,定量限分别为1.0μg/kg和0.5μg/kg。采用该方法对购自市场的30份全棉织物进行检测,其中1份检出苯胺,2份同时检出苯胺和二苯胺。

Based on the comparison of extraction efficiencies of different organic solvents and purification of solid phase extraction, high performance liquid chromatography （HPLC） with fluorescence detection was developed for the determination of trace aniline and diphenylamine in cotton fabric. In this case, acetonitrile/toluene （3/1） and Carb/PSA solid phase extraction column were used as the extraction solvent and cleaning column, and the sample was detected by high performance liquid chromatography with fluorescence detection at wavelength of 280 nm （λex） and 340nm （λem）. Mean recoveries of aniline and diphenylamine in three kinds of cotton fabrics at three spiked levels ranged from 97.3% to 103.5% and from 98.0% to 103.4%, respectively. The limits of detection for the two analytes were 0. 3 μg/kg and 0.2 μg/kg, respectively, and the limits of quantification were 1.0 μg/kg and 0. 5 μg/kg, respectively. The proposed method was used to monitor 30 cotton fabrics purchased from the market, among which one sample was found to contain aniline and two samples were found to contain both aniline and diphenylamine.