[1]赵玲,周蓓蕾,沈燕,等.气相色谱-串联质谱法测定鮰鱼、底泥、水体中18种多氯联苯[J].江苏农业学报,2017,(03):701-708.[doi:doi:10.3969/j.issn.1000-4440.2017.03.032]
　ZHAO Ling,ZHOU Bei-lei,SHEN Yan,et al.Using gas chromatography-tandem mass spectrometry（GC-MS/MS）for 18 polychlorinated biphenyls detection in water, sediment and fish (Ictalurus punctatus)[J].,2017,(03):701-708.[doi:doi:10.3969/j.issn.1000-4440.2017.03.032]
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气相色谱-串联质谱法测定鮰鱼、底泥、水体中18种多氯联苯()
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江苏农业学报[ISSN:1006-6977/CN:61-1281/TN]

卷:
期数:
2017年03期
页码:
701-708
栏目:
加工贮藏·质量安全
出版日期:
2017-06-30

文章信息/Info

Title:
Using gas chromatography-tandem mass spectrometry（GC-MS/MS）for 18 polychlorinated biphenyls detection in water, sediment and fish (Ictalurus punctatus)
作者:
赵玲1;2; 周蓓蕾2; 沈燕2; 董文斌2; 张迪骁2; 刘贤金2; 张存政2
（1.南京农业大学植物保护学院，江苏南京210095；2.江苏省农业科学院食品质量安全与检测研究所，江苏南京210014）
Author(s):
ZHAO Ling1;2; ZHOU Bei-lei2; SHEN Yan2; DONG Wen-bin2; ZHANG Di-xiao2; LIU Xian-jin2; ZHANG Cun-zheng2
(1.College of Plant Protection, Nanjing Agricultural University, Nanjing 210095, China;2.Institute of Food Safety and Inspection, Jiangsu Academy of Agricultural Sciences, Nanjing 210014, China)
关键词:
水; 底泥; 鮰鱼; 多氯联苯; 气相色谱-串联质谱
Keywords:
water; sediment; fish (Ictalurus punctatus); polychlorinated biphenyl; gas chromatography-tandem mass spectrometry
分类号:
X830.2
DOI:
doi:10.3969/j.issn.1000-4440.2017.03.032
文献标志码:
A
摘要:
建立了基于气相色谱-串联质谱法同时检测鮰鱼、底泥、水体中7种环境指示类、12种二噁英类多氯联苯（PCB）的定性定量分析方法。鮰鱼组织样品经液氮冷冻后粉碎处理，用二氯甲烷∶正己烷（体积比1∶1)提取，浓硫酸消解净化；底泥样品风干研磨过筛，水样品过滤，二氯甲烷提取，浓硫酸和弗罗里硅土柱净化，浓缩后正己烷定容。采用HP-5（30 m×0.32 mm×032 μm）毛细管柱分离，程序升温，质谱采用电子轰击电离源（EI），能量70 eV，以多反应监测模式（MRM）进行定性定量分析。7种环境指示类和12种二噁英类多氯联苯的平均回收率为73.16%～115.06%，相对标准偏差（RSD，n=5）为0.6%～93%，检出限为 040～060 μg/kg，测定限为100 μg/kg。该法简单，净化效果好，精密度高，可以准确检测水体、底泥、鱼体中18种PCB含量。
Abstract:
A method using gas chromatography - tandem mass spectrometry for multi-determination of 18 polychlorinated biphenyls (PCBs) including seven types of environment indicators and 12 types of coplanar in water, sediment and fish (Ictalurus punctatus) was developed. Fish tissue was dehydrated by liquid nitrogen, grounded, and extracted by the mixture solution of dichloromethane∶ hexane (V/V, 1∶1). Final extract was digested by concentrated sulfuric acid. Sediment sample was dried, filtered, and extracted by dichloromethane. Final extracts were digested by concentrated sulfuric acid, cleaned-up with Florida silica column, and resolved in hexane and ready for GC-MS/SM analysis. HP-5 flexible quartz capillary column（30 m×0.32 mm×032 μm）was used for the separation of 18 PCBs through temperature programming. Electron impact ion source (EI), 70 eV, and multiple reaction monitoring (MRM) model was set for the qualification and quantification in tandem mass spectrometry. The recoveries of spiked samples were 73.16%-11506% for 18 PCBs, with relative standard deviations (RSD, n=5) ranging from 0.6%-93%. The limits of detection were 0.40-060 μg/kg, and the lower limits was 100 μg/kg. This method is simple, and suitable for the analysis of PCBs residues in water, stediment and fish (Ictalurus punctatus).

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备注/Memo

备注/Memo:
收稿日期：2016-07-18 基金项目：江苏省农业科技自主创新资金项目[CX（15)1013] 作者简介：赵玲（1991-），女，河南邓州人，硕士，主要研究方向为农药残留与农产品质量安全检测。（Tel）025-84390401;（E-mail）zhaoheqiyun@163.com 通讯作者：张存政，（E-mail）zhcz2003@hotmail.com
更新日期/Last Update: 2017-06-29