食品科学

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超声波萃取-GPC净化-GC-ECD法测定鲍鱼不同组织中的多氯联苯

胡红美,郭远明,孙秀梅,郑元晟,钟 志,陈雪昌,刘 琴   

  1. 1.浙江省海洋水产研究所,浙江省海水增养殖重点实验室,浙江 舟山 316021;
    2.浙江海洋学院东海科学技术学院,浙江 舟山 316000
  • 出版日期:2013-12-25 发布日期:2014-01-03

Determination of PCBs in Different Tissues of Abalone by GC-ECD Following Ultrasonic Extraction and GPC Purification

HU Hong-mei,GUO Yuan-ming,SUN Xiu-mei,ZHENG Yuan-sheng,ZHONG Zhi,CHEN Xue-chang,LIU Qin   

  1. 1. Key Laboratory of Mariculture and Enhancement of Zhejiang Province, Marine Fishery Institute of Zhejiang Province,Zhoushan 316021, China;2. Donghai School of Science and Technology, Zhejiang Ocean University, Zhoushan 316000, China
  • Online:2013-12-25 Published:2014-01-03

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%和72.6%~91.4%,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。

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

Abstract:

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-hexane 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.

Key words: ultrasonic extraction, gel permeation chromatography (GPC), gas chromatography with electron capture detector (GC-ECD), different tissues of abalone, polychlorinated biphenyls (PCBs)