摘要
建立了测定鲍鱼不同组织（肌肉、内脏、整贝）样品中7种多氯联苯（PCBs）的气相色谱电子捕获检测方法（GC—ECD）。样品通过正己烷超声波萃取、凝胶渗透色谱初净化后，除肌肉部分样品，已经基本除杂干净，可直接上机分析；内脏部分和整贝需经佛罗里硅土固相萃取小柱进一步净化，再采用GC-ECD法检测，外标法定量。结果表明：7种PCBs在1．25～100μg／L质量浓度范围内，组分含量与峰面积呈线性相关，相关系数为0．9990-0．9999，检出限为0．04～0．06μg／kg。7种PCBs在肌肉部分、内脏部分、整贝中不同质量浓度水平的加标回收率分别为80．9％～105％、71．2％～92．3％3172．6％491．4％，相应的相对标准偏差分别为3．22％-6．80％、3．46％-7．01％、3．83％-6．86％（n=5）。本方法简单快速、基体干扰小、线性范围宽，灵敏度、准确度、精密度能满足鲍鱼不同组织中PCBs含量分析。
A simple, efficient, and sensitive method with low matrix interference for determination of 7 polychlorinated biphenyls （PCBs） in 3 different tissues of abalone using gas chromatography-electron capture detector （GC-ECD） has been developed. Muscle tissue samples were treated by ultrasonic extraction with n-bexane and gel permeation chromatography （GPC）. Further purification on a florisil solid phase extraction （SPE） column was needed for both viscera tissue and whole cowry samples before analysis. The linearity of the method ranged from 1.25 to 100 μg/L, with correlation coefficients ranging from 0.9990 to 0.9999. The limits of detection for 7 PCBs were 0.04-0.06 μg/kg. The recoveries of all the PCBs from muscle, viscera and whole cowry samples spiked at different concentrations were 80.9%-105%, 71.2%-92.3%, and 72.6%-91.4%, respectively, with relative standard deviations of 3.22%-6.80%, 3.46%-7.01%, and 3.83%-6.86% （n = 5）, respectively. This simple and rapid method had the advantages of low matrix interference, wide linear range and high sensitivity, accuracy and precision and thus could meet the requirements for the analysis of PCBs in different tissues of abalone.
出处
《食品科学》
EI
CAS
CSCD
北大核心
2013年第24期217-221,共5页
Food Science
基金
浙江省科技计划项目(2012F30021
2012F30026)
浙江省重点科技创新团队项目(2010R50028)
关键词
超声波萃取法
凝胶渗透色谱法
气相色谱电子捕获检测法
鲍鱼不同组织
多氯联苯
ultrasonic extraction
gel permeation chromatography （GPC）
gas chromatography with electron capturedetector（GC-ECD）
differenttissuesofabalone
polychlorinatedbiphenyls（PCBs）
