【摘要】 建立了加速溶剂萃取(ASE)-气相色谱/电子捕获(GC/ECD)检测皮革中五氯苯酚(PCP)的方法。通过萃取剂选择实验和正交实验,确定了加速溶剂萃取的最佳参数:正己烷为萃取溶剂,萃取温度120℃,静态萃取时间3 min,循环次数3次,氮气吹扫时间80 s。提取液经浓缩、净化、乙酸酐衍生后以气相色谱法测定,以标准物质保留时间定性,外标法定量。结果表明,所建立方法的线性范围为0.02～2 mg/L,相关系数>0.999,方法的检出限为0.004 mg/kg。标准加入回收率为96.9%～98.3%,RSD<5.68%(n=7),方法快速、简便易行、灵敏度高,可作为测定皮革中PCP的新方法。更多还原

【Abstract】 A method of accelerated solvent extraction(ASE) and gas chromatography with electron capture detector(GC/ECD) was developed for the determination of pentachlorophenol(PCP) in leather.The condition parameters of ASE were optimized,which were hexane as extraction solvent,extraction temperature 120 ℃,static extraction time 3 min,3 cycles,nitrogen purge time 80 s.The extract was concentrated,purified,acetic anhydride derivatives,and then analyzed by gas chromatography.Qualitative and quantitative analysis was carried out on retention time of PCP by external standard method.The mass concentration of PCP was a linear range of 0.1~20 mg/L with good correlation coefficients(r>0.999),and the detection limit of this method for PCP was 0.004 mg/kg.The mean recoveries were 96.9%~98.3%,RSD<5.68%(n=7),The proposed method was fast,simple,sensitive,therefore it is suitable for determining PCP in leather.更多还原