Chen Ligang, Jin Haiyan, Wang Liguang, Sun Lei, Xu Haoyan, Ding Lan, Yu Aimin, Zhang Hanqi
College of Chemistry, Jilin University, 2699 Qianjin Street, Changchun 130012, China.
J Chromatogr A. 2008 May 23;1192(1):89-94. doi: 10.1016/j.chroma.2008.03.037. Epub 2008 Mar 19.
An on-line method was developed for the extraction, derivatization and determination of formaldehyde in textile samples. Formaldehyde was first extracted with water by ultrasound assisted, and directly introduced into a derivatization column which was packed with a moderately sulfonated cation-exchange resin. The resin used as solid support for the derivatization was charged with 2,4-dinitrophenylhydrazine (DNPH) previously. The formaldehyde DNPH derivative was eluted with the chromatographic mobile phase into an analytical column for the separation, and then monitored by UV detector. The maximum extraction yield was achieved when the extraction vessel was located at 10mm from the ultrasonic source and 10mg textile sample was extracted with 5mL pure water at a flow rate of 1.0mLmin(-1) at 50 degrees C. The detection limit of the proposed method was 0.06mgkg(-1). This method was applied to the determination of formaldehyde in different textile samples, and compared with the state standard method (off-line spectrophotometry) used in China. The similar contents of formaldehyde were obtained for most samples by the two methods, but little higher for some samples obtained by the proposed method. The average relative standard deviation (RSD) obtained by the on-line method was 3.2% which is lower than 29.5% obtained by the standard method.
建立了一种在线提取、衍生化和测定纺织品样品中甲醛的方法。首先通过超声辅助用水提取甲醛，然后直接将其引入填充有适度磺化阳离子交换树脂的衍生化柱中。用作衍生化固体支持物的树脂预先用2,4 -二硝基苯肼（DNPH）进行了装填。甲醛DNPH衍生物用色谱流动相洗脱至分析柱进行分离，然后用紫外检测器进行监测。当萃取容器距离超声源10mm，在50℃下以1.0mLmin(-1)的流速用5mL纯水萃取10mg纺织品样品时，可获得最大萃取率。该方法的检测限为0.06mgkg(-1)。将该方法应用于不同纺织品样品中甲醛的测定，并与中国使用的国家标准方法（离线分光光度法）进行了比较。两种方法对大多数样品获得的甲醛含量相似，但该方法对一些样品获得的含量略高。在线方法获得的平均相对标准偏差（RSD）为3.2%，低于标准方法获得的29.5%。
