气相色谱-负化学电离源质谱法测定鱼油中16种多氯联苯

doi:10.3724/SP.J.1123.2015.04010

色谱 ›› 2015, Vol. 33 ›› Issue (8): 878-884.DOI: 10.3724/SP.J.1123.2015.04010

气相色谱-负化学电离源质谱法测定鱼油中16种多氯联苯

王丽¹, 李书书², 张展¹, 王守林², 李磊¹

1. 南京医科大学公共卫生学院卫生检验学系, 江苏南京 211166;
2. 南京医科大学公共卫生学院职业卫生与环境卫生学系, 江苏南京 211166

收稿日期:2015-04-07 出版日期:2015-08-08 发布日期:2015-07-27
通讯作者: 李磊
基金资助:
江苏省高校优势学科建设工程项目(PAPD2010).

Determination of 16 polychlorinated biphenyls in fish oil by gas chromatography-negative ion chemical ionization-mass spectrometry

WANG Li¹, LI Shushu², ZHANG Zhan¹, WANG Shoulin², LI Lei¹

1. Department of Hygienic Analysis and Detection, School of Public Health, Nanjing Medical University, Nanjing 211166, China;
2. Department of Occupational Health and Environmental Health, School of Public Health, Nanjing Medical University, Nanjing 211166, China

Received:2015-04-07 Online:2015-08-08 Published:2015-07-27

摘要/Abstract

摘要：

建立了气相色谱-负化学电离源质谱(GC-NCI-MS)同时测定鱼油中16种多氯联苯(PCBs)的方法。鱼油样品经正己烷提取和浓硫酸净化,在选择离子监测模式下进行GC-NCI-MS检测。所检测的PCBs在0.01~10 μg/L范围内呈现良好的线性关系(r>0.99),定量限(S/N=10)在3~67 pg/g之间。基质加标回收率为62.3%~121.8%,相对标准偏差(n=3)≤12%。相比传统的多种填料固相萃取前处理法,本方法样品处理简单快速,有机溶剂使用量少,具有较好的抗基质干扰能力和较高的灵敏度,适用于鱼油中痕量共平面多氯联苯及常见指示性多氯联苯等的同时检测。

关键词: 共平面多氯联苯, 气相色谱-负化学电离源质谱, 鱼油, 指示性多氯联苯

Abstract:

An analytical method for the simultaneous determination of 16 polychlorinated biphenyls (PCBs) in fish oil was developed. PCBs were extracted from fish oil with n-hexane, purified by sulfuric acid and determined by using gas chromatography-negative ion chemical ionization-mass spectrometry (GC-NCI-MS) in selected ion-monitoring (SIM) mode. A good linear relationship (r>0.99) was observed with the PCBs concentrations from 0.01 μg/L to 10 μg/L, and the limits of quantification (LOQ, S/N=10) were between 3 pg/g and 67 pg/g for different kinds of PCBs. The average recoveries ranged from 62.3% to 121.8% with the relative standard deviations (RSDs, n=3) smaller than 12%. Compared with the traditional pre-treatment of multiple material solid phase extraction, this new method is simple, rapid and less organic solvent usage. Meanwhile the method has good selectivity and sensitivity, and it is suitable for the determination of multiple trace PCBs in fish oil.

Key words: coplanar polychlorinated biphenyls (co-PCBs), fish oil, gas chromatography-negative ion mode of chemical ionization-mass spectrometry (GC-NCI-MS), indicator polychlorinated biphenyls

中图分类号:

O658

王丽, 李书书, 张展, 王守林, 李磊. 气相色谱-负化学电离源质谱法测定鱼油中16种多氯联苯[J]. 色谱, 2015, 33(8): 878-884.

WANG Li, LI Shushu, ZHANG Zhan, WANG Shoulin, LI Lei. Determination of 16 polychlorinated biphenyls in fish oil by gas chromatography-negative ion chemical ionization-mass spectrometry[J]. Chinese Journal of Chromatography, 2015, 33(8): 878-884.

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气相色谱-负化学电离源质谱法测定鱼油中16种多氯联苯

Determination of 16 polychlorinated biphenyls in fish oil by gas chromatography-negative ion chemical ionization-mass spectrometry

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