高效液相色谱荧光法测定印染废水中的二苯胺

Determination of diphenylamine in dyeing effluent by high performance liquid chromatography with fluorescence detection

建立了印染废水中微量二苯胺的高效液相色谱荧光检测方法。样品经HLB固相萃取小柱净化、浓缩后,在Kromasil C18色谱柱上以水/乙腈（体积比20/80）为流动相进行分离,采用荧光检测器检测,检测波长λex为265 nm,λem为350 nm。二苯胺在5.0~500.0μg/L范围内具有良好的线性关系,相关系数〉0.999,回收率为92.3%~104.2%,相对标准偏差（RSD）为1.2%~4.1%,方法的定量检出限（LOQ）为2.5μg/L。通过试验条件优化建立的方法干扰少、灵敏度高,适用于印染废水中二苯胺的检测。

A method for the determination of trace diphenylamine in dyeing effluent by high performance liquid chromatography coupled with fluorescence （HPLC-FL） detection was established. After the sample was cleaned and concentrated by a HLB solid-phase extraction （SPE） cartridge, the separation was performed on a Kromasil C18 column by the mobile phase of water/acetonitrile （20/80, V/V）. The detection was carried out by HPLC-FL at 265 nm （λex） and 350 nm （λem）. Calibration curve was linear within the range of 5.0~500.0 μg/L with the correlation coefficient of more than 0.999, the extraction recovery was 92.3%-104.2%, the relative standard deviation （RSD） was 1.2% -4.1%, and the limit of quantification （LOQ） was 2.5 μg/L, The developed method was less interference and high sensitivity by optimizing the experimental conditions, and suitable for the satisfactory determination of diphenylamine in dyeing effluent.