加速溶剂萃取-高效液相色谱法测定皮革和纺织品中含氯苯酚的含量

Determination of Chlorophenols in Leathers and Textiles by Accelerated Solvent Extraction and High Performance Liquid Chromatography

建立了测定皮革和纺织品中含氯苯酚的高效液相色谱/二极管阵列检测器(HPLC/DAD)分析方法。采用加速溶剂萃取法萃取不同类型的皮革和纺织品样品,以正己烷为提取剂,在10.34MPa和120℃下静态循环提取3次,提取液经氮吹仪浓缩近干,以正己烷溶解并定容;采用C18柱,以乙腈/0.5%乙酸溶液为流动相,DAD波长为214nm进行高效液相色谱分离与分析。结果表明:四氯苯酚和五氯苯酚质量浓度在0.1～20mg/L范围内具有良好的线性关系(r>0.9999);平均回收率在96.0%～101.5%之间;相对标准偏差为0.50%～5.5%(n=7);方法的检出限为0.02mg/kg,符合欧盟指令0.05mg/kg的限量规定。本方法高效、简便、自动化程度高,准确可靠,是一种可同时快速测定皮革和纺织品中含氯苯酚的新方法。

A method was developed for the determination of chlorophenols （tetrachlorophenol and pentachlo-rophenol） in leathers and textiles by accelerated solvent extraction （ASE） and high performance liquid chromatography with diode array detection （HPLC/DAD） .The crushed samples were extracted using ASE with n-hexane,and then the chlorophenols were eluted on a C18 column with acetonitrile and 0.5% acetic acid solution,which were detected by DAD at λ214 nm.Qualitative and quantitative analysis was carried out by retention time of chlorophenols and external standard method.The mass concentration of tetrachlorophenol and pentachlorophenol has a linear range of 0.1-20 mg/L with good correlation coefficients （r0.9999） ; The mean recoveries were 96.0%-101.5% ,with the relative standard deviation （RSD） of 0.50%-5.5% （n=7） ,and the detection limit of this method for chlorophenols was 0.02 mg/kg.