固相萃取净化-气相色谱-负化学源质谱法测定近岸海洋环境中的甲氧基多溴联苯醚

doi:10.3785/j.issn.1008-9497.2022.03.012

浙江大学学报（理学版）

2022, Vol. 49

Issue (3): 344-353 DOI: 10.3785/j.issn.1008-9497.2022.03.012

海洋科学

固相萃取净化-气相色谱-负化学源质谱法测定近岸海洋环境中的甲氧基多溴联苯醚

郜文^1,²,孙秀梅²(

),金衍健²,郝青²,傅宇^1,²,叶茂盛^1,²,杨承虎²,郭远明²

^1.浙江海洋大学海洋与渔业研究所，浙江舟山 316021
^2.浙江省海洋水产研究所浙江省海洋渔业资源可持续利用技术研究重点实验室，浙江舟山 316021

Determination of methoxypolybrominated diphenyl ethers in the coastal marine environment using solid-phase extraction and gas chromatography coupled with negative chemical ionization mass spectrometry

Wen GAO^1,²,Xiumei SUN²(

),Yanjian JIN²,Qing HAO²,Yu FU^1,²,Maosheng YE^1,²,Chenghu YANG²,Yuanming GUO²

^1.Institute of Marine and Fisheries，Zhejiang Ocean University，Zhoushan 316021，Zhejiang Province，China
^2.Key Laboratory of Sustainable Utilization of Technology Research for Fishery Resource of Zhejiang Province，Zhejiang Marine Fisheries Research Institute，Zhoushan 316021，Zhejiang Province，China

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摘要：

甲氧基多溴联苯醚（methoxypolybrominated diphenyl ethers， MeO-PBDEs）广泛存在于生物体和海洋环境。以象山海域的生物体和沉积物为样本，采用固相萃取净化-气相色谱-负化学源质谱法，检测了6种MeO-PBDEs，结果显示，当目标分析物浓度为0.1~20.0 μg?L^-1时，线性关系良好（R²>0.999），检出限为0.13~0.22 μg?kg^-1，定量限为0.42~0.72 μg?kg^-1，实际样品的平均回收率为71.2%~116.2%。MeO-PBDEs的分布状况调查结果显示，藻类样品中仅检出6-MeO-BDE-47，且浓度较低，其他生物体中检出3种MeO-PBDEs，检出率为31.3%，浓度为0.21~2.72 μg?kg^-1。沉积物中无MeO-PBDEs被检出。

关键词： 甲氧基多溴联苯醚; 气相色谱-负化学源质谱; 固相萃取净化; 海洋环境

Abstract:

Methoxypolybrominated diphenyl ethers (MeO-PBDEs) were widely present in marine organisms and the marine environment. An analytical method of six methoxypolybrominated diphenyl ethers for biological samples and sediment samples from Xiangshan Sea area using solid-phase extraction and gas chromatography coupled with negative chemical ionization mass spectrometry was developed and optimized. The developed method exhibited satisfying linearity in the range of 0.1-20.0 μg?L^-1 (R²>0.999). The detection limit (LOD) and limit of quantitation (LOQ) for MeO-PBDEs were 0.13-0.22 μg?kg^-1 and 0.42-0.72 μg?kg^-1 respectively. The spiked recovery was 71.2%-116.2%. The method was applied to the analysis of marine organisms and sediments collected from Xiangshan sea area. All kinds of MeO-PBDEs were not detected in sediment samples. Only 6-MeO-BDE-47 was detected in algae samples with low concentration. Three MeO-PBDEs were detected in other biological samples, and the ratio of detection was 31.3% with a concentration range of 0.21-2.72 μg?kg^-1MeO-PBDEs were not detected in sediment samples.

Key words: methoxypolybrominated diphenyl ethers gas chromatography-negative chemical ionization mass spectrometry solid-phase extraction marine environment

收稿日期: 2021-01-21 出版日期: 2022-05-24

CLC:

X 834

基金资助: 国家自然科学基金资助项目(21407127);浙江省科技厅项目(2018C37024)

通讯作者: 孙秀梅 E-mail: sunxiumei82@sina.com

作者简介: 郜文（1995—），ORCID：https：//orcid.org/0000-0001-6354-8645，女，硕士研究生，主要从事水域环境管理与评估研究.

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引用本文:

郜文,孙秀梅,金衍健,郝青,傅宇,叶茂盛,杨承虎,郭远明. 固相萃取净化-气相色谱-负化学源质谱法测定近岸海洋环境中的甲氧基多溴联苯醚[J]. 浙江大学学报（理学版）, 2022, 49(3): 344-353.

Wen GAO,Xiumei SUN,Yanjian JIN,Qing HAO,Yu FU,Maosheng YE,Chenghu YANG,Yuanming GUO. Determination of methoxypolybrominated diphenyl ethers in the coastal marine environment using solid-phase extraction and gas chromatography coupled with negative chemical ionization mass spectrometry. Journal of Zhejiang University (Science Edition), 2022, 49(3): 344-353.

链接本文:

https://www.zjujournals.com/sci/CN/10.3785/j.issn.1008-9497.2022.03.012 或 https://www.zjujournals.com/sci/CN/Y2022/V49/I3/344

表1 象山海域生物样品信息

图1 6种MeO-PBDEs标准品的总离子流色谱（20 μg∙L-1）

图2 不同提取方式对沉积物样品中MeO-PBDEs 回收率的影响（n=3）

图3 不同固相萃取柱对生物样品中MeO-PBDEs回收率的影响（n=3）

图4 不同酸化时间对生物样品中MeO-PBDEs回收率的影响（n=3）

表2 线性相关系数、检出限和定量限

表3 不同加标水平下MeO-PBDEs在4种生物样品中的加标回收率与RSD

图5 象山海域鱼类样品中检出的MeO-PBDEs浓度

图6 象山海域甲壳类样品中检出的MeO-PBDEs浓度

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