微波提取联合液相色谱测定皮革中五氯苯酚含量的方法研究

Study on the Determination Method of Pentachlorophenol Content in Leather by Microwave Extraction Combined with Liquid Chromatography

探讨了一种前处理采用微波提取、后续使用液相色谱测定皮革中五氯苯酚含量的方法。对液相色谱流动相的选择、流速等条件进行了优化,绘制了五氯苯酚(PCP)的标准曲线,测定了方法的回收率、检出限和精密度。结果表明:当液相色谱的流动相为乙腈/p H 2.0磷酸水溶液,流速为1m L/min,且采用梯度洗脱的方式进行试验时,绘制的PCP标准曲线线性良好,相关系数为0.9998;方法的回收率≥95%,检出限为0.25mg/kg,12次平行试验的相对标准偏差(RSD)为1.3%。基于微波提取能够快速、高效地完成皮革中五氯苯酚含量的检测。

The article explored a kind of method about determination of pentachlorophenol in leather which pretreated by microwave extraction and subsequently measured using liquid chromatographic（HPLC）. The selection of HPLC mobile phase, flow rate conditions of HPLC were optimized and the standard curve of pentachlorophenol（PCP）via liquid chromatography was drawn.The recovery rate of the method, detection limit of the method and precision of the method were measured. The research results indicated that as the acetonitrile/aqueous solution of phosphoric acid（p H 2.0）, HPLC mobile phase were the best compared with others. The standard curve linear of PCP via liquid chromatography was good（the correlation coefficient of 0.9998）, the recovery rate was95% or more, the method detection limit was 0.25 mg/kg, the RSD of 12 times parallel test was1.3% when the flow rate of HPLC mobile phase was 1 m L/min and the test was performed using gradient elution. The results also indicated that the test was completed quickly when determination of pentachlorophenol in leather with microwave extraction and HPLC.