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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。
A high performance liquid chromatographic method for the determination of aniline and diphenylamine in cotton fabrics was established. The cotton fabric was purified on a Carb / PSA SPE cartridges using acetonitrile / toluene (3/1, V / V) as extractant and water / water on a Kromasil C18 column (250 mm × 4.6 mm id, Acetonitrile (25/75, V / V) as the mobile phase. The fluorescence detection wavelength λex was 280 nm and λem was 340 nm. The results showed that the average recoveries of aniline and diphenylamine at the three spiked levels were 97.3% -103.5% and 98.0% -103.4%, respectively, and the relative standard deviations were 1.4% -4.2% and 0.98%, respectively. ~ 4.7%. The detection limits of the method were 0.3μg / kg and 0.2μg / kg respectively. The limits of quantification were 1.0μg / kg and 0.5μg / kg, respectively. Using this method, 30 cotton fabrics from the market were tested, of which 1 was aniline and 2 were aniline and diphenylamine simultaneously.