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机构地区:[1]浙江工商大学食品与生物工程学院,杭州310012 [2]浙江省地质矿产研究所,杭州310007
出 处:《中国食品学报》2012年第2期151-157,共7页Journal of Chinese Institute Of Food Science and Technology
摘 要:目的:建立同时检测蔬菜中19种多氯联苯(PCBs)的气相色谱-质谱-选择离子监测(GC-MS-SIM)分析方法。方法:将样品经丙酮/正己烷(体积比1:1)索氏提取、浓硫酸及Florisil固相萃取柱(SPE)净化、氮吹浓缩后,用GC-MS测定。结果:各种PCBs得到较好分离。经方法学验证,19种PCBs标准曲线的线性相关系数在0.99859~0.99962之间,方法检出限0.04~0.43μg/kg(S/N=3),目标化合物加标回收率为87.5%~106.8%,相对标准偏差(RSD,n=5)为1.6%~6.7%。结论:该方法灵敏、准确、稳定,能满足蔬菜样品中痕量多氯联苯的测定。Objective: A method for simultaneous determination of 19 polychlorinated biphenyls (PCBs) in vegetables by gas chromatography-mass spectrometry-sleetive ion mode (GC-MS-SIM) was developed. Method: Samples were extract- ed with n-hexane/actone(V/V 1:1) by Soxhlet extraction and purified with sulfuric acid and a Florisil solid phase extrac- tion column(SPE,1 g/6 mL) and concentrated by N2 blowing. The analysis was carried out by using GC-MS with electron impact (El) source. Results: The experimental results showed a good linear relationship between the peak area and the concentration (r=0.99859-0.99962), and the average recoveries ranged from 87.5% to 106.8% with the relative standard deviation (RSD, n=5) range from 1.6% to 6.7%, the limits of detection are between 0.04 and 0.43 μg/kg. Conclusion: The method provides the advantages of high sensitivity and accuracy as well as repeatability and meet the requirements for the determination of PCBs in vegetables.
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