【摘要】 建立了气相色谱-质谱联用法测定皮革中2-氯联苯(PCB 1)、2,2’-二氯联苯(PCB 4)、2,4,4’-三氯联苯(PCB 28)、2,2’,5,5’-四氯联苯(PCB 52)、2,2’,4,5,5’-五氯联苯(PCB 101)、2,2’,3,4,4’,5’-六氯联苯(PCB138)、2,2’,3,4,4’,5,5’-七氯联苯(PCB 180)、2,2’,3,3’,4,4’,5,5’-八氯联苯(PCB 194)、2,2’,3,3’,4,4’,5,5’,6-九氯联苯(PCB 206)、十氯联苯(PCB 209)等10种多氯联苯的方法。试样采用叔丁基甲醚超声提取,提取液浓缩后用Florisil小柱净化,净化液浓缩后用正己烷定容。10种多氯联苯经HP-5MS石英毛细管柱分离,进行气相色谱-质谱联用仪分析,全扫描定性,选择离子定量。结果表明,10种多氯联苯线性范围为0.5~10μg/m L,r≥0.9990,检出限为0.5 mg/kg,回收率为73.7%~113.3%,RSD≤5.7%(n=6)。方法简便、快速、准确,稳定可靠,适用于皮革中10种多氯联苯的同时检测。更多还原

【Abstract】 A GC-MS method was developed for the determination of 10 polychlorinated biphenyls, 2-chlorobiphenyl(PCB1), 2,2’-dichlorobiphenyl(PCB 4), 2,4,4’-trichlorobiphenyl(PCB 28), 2,2’,5,5’-tetrachlorobiphenyl(PCB 52), 2,2’,4,5,5’-chlorobiphenyl(PCB 101), 2,2’,3,4,4’,5’-chlorobiphenyl(PCB 138), 2,2’,3,4,4’,5,5’-chlorobiphenyl(PCB 180), 2,2’,3,3’,4,4’,5,5’-chlorobiphenyl(PCB 194), 2,2’,3,3’,4,4’,5,5’,6-chlorobiphenyl(PCB 206) and decachlorobiphenyl(PCB 209) in leather. The samples were extracted with tert-butylmethyl ether in ultrasonic bath. The extracted products was concentrated and then cleaned up with Florisil column. The cleaned fluid was concentrated and then volumed with hexane. 10 polychlorinated biphenyls were separated in HP-5 MS quartz capillary column and fully scanned for qualitative analysis and selected scanned for quantitative analysis by GC/MS. The calibration curves showed good linear relationship in the range of 0.5~10 μg/m L. The correlation coefficients were more than 0.9990. The detection limits were 0.5 mg/kg.The recoveries ranged from 73.7% to 113.3% with relative standard deviations lower than 5.7% when n =6. The method was simple, rapid, accurate and was stable, reproducible for the determination of 10 polychlorinated biphenyls in leather.更多还原