高效液相色谱法同时测定纺织品中四氯苯酚同分异构体及五氯苯酚和邻苯基苯酚

Simultaneous Determination of Tetrachlorophenol,Pentachlorophenol,and Orthophenylphenol in Textiles by High Performance Liquid Chromatography

建立了高效液相色谱法同时测定纺织品中四氯苯酚同分异构体（2,3,4,5-TeCP、2,3,4,6-TeCP、2,3,5,6-TeCP）及五氯苯酚（PCP）和邻苯基苯酚（OPP）的分析方法。样品经甲醇超声提取、浓缩后,采用Symmetry C18色谱柱,以甲醇-10mmol/L乙酸铵溶液为流动相,梯度洗脱,二极管阵列检测器210nm检测。结果表明：三种TeCP同分异构体及PCP、OPP在0.1~20mg/L范围内具有良好的线性关系,相关系数为0.9994~0.9998,样品加标回收率为87.2%~109%,相对标准偏差为0.92%~4.50%,方法的最低检测浓度分别为0.05、0.10、0.05、0.05、0.05mg/kg。该方法高效、简便、准确可靠,可实现现行法规所要求的纺织品中苯酚类物质的同时测定。

A high performance liquid chromatograph（HPLC）method was established for the simultaneous separation and determination of Tetrachlorophenol（2,3,4,5-TeCP、2,3,4,6-TeCP、2,3,5,6-TeCP）,pentachlorophenol（PCP）and orthophenylphenol（OPP）in textiles.The samples were dissolved by methanol and extracted by ultrasonic extraction.The extract was first concentrated and filtrated,and then the separation of analytes was preformed on Symmetry C18（250×4.6 mm i.d.,5μm）with methanol and 10mmol/L NH4Ac（pH=6.6）as mobile phase using gradient elution at a flow-rate of 1.0mL/min.After that,the extract was detected with a photodiode array detector at 210 nm.The result indicated that the five analytes were completely separated in 30 min.The calibration curves showed good linearity in the range of 0.1-20mg/L with correlation coefficients of 0.9994-0.9998.The recoveries of this method were in the range of 87.2%-109% with RSD below 4.50%（n=3）,and the detection limits of this method for 2,3,4,5-TeCP,2,3,4,6-TeCP,2,3,5,6-TeCP,PCP,OPP were 0.05,0.01,0.05,0.05,0.05mg/kg,respectively.