引用本文:
石银俊, 周衍霄, 朱国华, 李沐霏, 巩宏平, 刘劲松. 同位素稀释气相色谱-高分辨质谱法测定土壤和沉积物中20种多溴联苯[J]. 环境化学, 2018, 37(9): 1994-2001
SHI Yinjun, ZHOU Yanxiao, ZHU Guohua, LI Mufei, GONG Hongping, LIU Jinsong. Determination of 20 polybrominated biphenyls in soil and sediment by isotope dilution gas chromatography-high resolution mass spectrometry[J]. Environmental Chemistry, 2018, 37(9): 1994-2001

同位素稀释气相色谱-高分辨质谱法测定土壤和沉积物中20种多溴联苯
石银俊1, 周衍霄1, 朱国华2, 李沐霏2, 巩宏平2, 刘劲松1,2
1. 浙江工业大学, 化学工程学院, 杭州, 310014;
2. 浙江省环境监测中心, 杭州, 310015
摘要:
本文建立了土壤和沉积物中20种多溴联苯的同位素稀释气相色谱-高分辨质谱分析方法.样品经索氏提取、多层硅胶柱净化,采用气相色谱-高分辨质谱分析,各组分在10 -1000 ng·mL-1范围内线性良好,平均相对响应因子(RRF)的偏差在2.9%-15.1%之间.方法检出限在2.57-135 ng·kg-1之间,批间偏差为1.0%-15.1%.低、中、高的3个加标水平实际样品平均回收率为64.8%±5.5%-156%±7.1%.该方法可用于土壤和沉积物中痕量多溴联苯的检测.
关键词:    多溴联苯    同位素稀释    气相色谱-高分辨质谱    土壤和沉积物    持久性有机污染物(POPs)   
Determination of 20 polybrominated biphenyls in soil and sediment by isotope dilution gas chromatography-high resolution mass spectrometry
SHI Yinjun1, ZHOU Yanxiao1, ZHU Guohua2, LI Mufei2, GONG Hongping2, LIU Jinsong1,2
1. Zhejiang University of Technology, Hangzhou, 310014, China;
2. Zhejiang Environmental Monitoring Center, Hangzhou, 310015, China
Abstract:
A simultaneous extraction and determination method for 20 polybrominated biphenyls (PBBs) in soil and sediment was developed based on isotope dilution gas chromatography-high resolution mass spectrometry (GC-HRMS). Under the optimized extraction, clean-up and analysis conditions, the results showed that the linear range of 20 PBBs was between 10 to 1000 ng·mL-1, and the relative deviation of the relative response factor (RRF) was between 2.9% to 15.1%. The method detection limits (MDLs) ranged from 2.57 ng·kg-1 to 135 ng·kg-1. The recoveries of the 20 PBBs spiked in soil and sediment samples at low, medium and high levels were 64.8%±5.5% to 156%±7.1%. This method can be efficiently applied to the determination of trace PBBs in soil and sediment.
Key words:    polybrominated biphenyls(PBBs)    isotope dilution    gas chromatography-high resolution mass spectrometry(GC-HRMS)    soil and sediment    POPs   
收稿日期: 2017-11-13
基金项目: 浙江省环保科研基金(2017A005,2017A006)资助.
刘劲松,Tel:0571-89975336,E-mail:liu70923@163.com
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