高效液相色谱法测定家具中释放的15种醛酮类化合物的含量

Determination of 15 Aldehydes and Ketones Liberated from Furnitures by HPLC

将装有2,4-二硝基苯肼(DNPH)的采样管的两端分别安装在气候箱采样口和恒流空气采样器上,调节其空气流量为0.50L·min-1,采样时间为20min,测定气候箱的空白值。打开箱门后迅速将欲检测其释放的醛酮有机污染物的样品(如家具等)置于箱内,关闭箱门,开始计时,随即用上述采样管采集气候箱第24h的空气样品。空气样品中的醛酮有机污染物被采样管中的DNPH所吸附,并反应生成稳定的腙类衍生物。将采样管移置在SPE仪上,用乙腈5mL将上述腙类衍生物洗脱,所得洗脱液用于高效液相色谱法分析,用二极管阵列检测器(PDA)检测,检测波长为360nm。结果表明:15种醛酮-DNPH在0.20～20mg·L-1内与其对应的色谱峰面积之间呈线性关系,检出限(3s)在0.011～0.054μg·m-3之间。按照标准加入法进行加标回收试验,15种醛酮类化合物的回收率在84.6%～113%之间,测定值的相对标准偏差(n=6)在0.40%～3.6%之间。

Two ends of the 2,4-dinitrophenylhydrazine(DNPH)sampling tube were connected separately with the outlet of climatic chamber and the suction tube of the constant current air sampler,which was adjusted to have an air flow-rate of 0.50 L·min^-1,and a sampling time of 20 min.Blank test was made as the chamber is empty.The chamber was opened and the testing sample,such as the furnitures which may liberate those organic pollutants of aldehydes and ketones,should be put into the chamber as quick as possible and the chamber was closed immediately.Sampling of the air from the climatic chamber was started at this moment.Air sample at the 24 th hour was collected for analysis.The organic pollutants in air sample were adsorbed by DNPH and transformed to stable hydrazone derivatives,which were eluted from the sampling tube by SPE with 5 mL of acetonitrile,and the eluate obtained was analyzed by HPLC and the pollutants of aldehydes and ketones were separated by HPLC and detected by PDA detector at the wavelength of 360 nm.As shown by the results,linear relationships between values of peak area and mass concentration of 15 kinds of aldehyde-DNPH and ketone-DNPH were found in the same range of0.20-20 mg·L^-1,with detection limits(3 s)in the range of 0.011-0.054μg·m^-3.Test for recovery was made by standard addition method,giving results in the range of 84.6%-113%,and RSDs(n=6)were found in the range of 0.40%-3.6%.