磺化净化-GC-MS法测定皮革中8种多氯联苯
Determination of 8 Polychlorinated Biphenyls in Leather by Sulfonation Purification and Gas Chromatography-mass Spectrometry
作者：周良春, 张晓飞, 王睿, 马俊辉, 李双琦, 胡伟
Author：ZHOU Liangchun, ZHANG Xiaofei, WANG Rui, MA Junhui, LI Shuangqi, HU Wei
收稿日期：2019-06-13 年卷（期）页码：2020,30(1):43-47
期刊名称：皮革科学与工程
Journal Name：Leather Science and Engineering
关键字：气相色谱-质谱法,皮革,多氯联苯,超声提取,磺化净化,
Key words：gas chromatography-mass spectrometry,leather,polychlorinated biphenyls,ultrasonic extraction,sulfonation purification,
基金项目：
中文摘要
建立了磺化净化-气相色谱-质谱法测定皮革中2,2',5-三氯联苯（PCB18）、2,4,4'-三氯联苯（PCB28）、 2,2',5,5'-四氯联苯（PCB52）、2,2',4,5,5'-五氯联苯（PCB101）、2,3',4,4',5-五氯联苯（PCB118）、2,2',3,4,4',5'-六氯联苯（PCB138）、2,2',4,4',5,5'-六氯联苯（PCB153）和2,2',3,4,4',5,5'-七氯联苯（PCB180）8种多氯联苯含量的方法。分别讨论了提取溶剂,提取温度和提取时间对8种多氯联苯回收率的影响。将样品剪成约5 mm×5 mm左右的细小颗粒混匀后,用10 mL正己烷,30 ℃超声20 min,提取液用浓硫酸净化,上清液用0.45 μm的滤膜过滤后,用DB-5MS 石英毛细管色谱柱( 30 m×0.25 mm×0.25 μm) 分离,采用GC-MS选择离子检测,外标法定量。结果表明：在0.05~1.0 mg/L范围内,线性良好,相关系数均大于0.999,方法检出限为0.2 mg/kg;加标平均回收率在92.0 %~108.1 %之间,RSD≤4.5 %。该方法快速、准确,重现性好,适用于皮革及其制品中8种多氯联苯含量的同时测定。
英文摘要
One method was developed for the determination of 8 polychlorinated biphenyls ( including 2,2',5-trichlorobiphenyl (PCB18), 2,4,4'-trichlorobiphenyl (PCB28), 2,2',5,5'-tetrachlorobiphenyl (PCB52), 2,2',4,5,5'-pentachlorobiphenyl (PCB101), 2,3',4,4',5-pentachlorobiphenyl (PCB118), 2,2',3,4,4', 5'-hexachlorobiphenyl (PCB138), 2,2',4,4',5,5'-hexachlorobiphenyl (PCB153), and 2,2',3,4,4',5,5'-heptachlorobiphenyl (PCB180)) in leather by sulfonation purification and gas chromatography-mass spectrometer(GC-MS). The effects of recoveries of 8 polychlorinated biphenyls by different extraction solvent, extraction temperature and extraction time were discussed respectively.The samples were cut to 5 mm × 5 mm sieve, extracted with 10 mL n-hexane, and ultrasound at 30 ℃ for 20 minutes.The extract solution was purified with concentrated sulfuric acid. The supernatant was filtered with 0.45um filter membrane and the polychlorinated biphenyls were separated by DB-5MS quartz capillary column(30 m ×0.25 mm, 0.25 μm).The samples were detected by GC-MS and quantified by external standard method.The results showed that the correlation coefficients r were more than 0.999 in the range of 0.05-1.0 mg/L.The limit of detection was 0.2 mg/kg. The average recovery rate ranged from 92.0 % to 108.1%, and the relative standard deviations(n=6) were less than 4.5 %.The method was rapid, accurate and reproducible, and could be suitable for the determination of 8 polychlorinated biphenyls in leather and its products.
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