在线固相萃取-高效液相色谱-电感耦合等离子体质谱法同时测定血清中多溴二苯醚及其羟基代谢产物

引用本文: 金津, 宋善军, 彭子娟, 郭峰, 李彭辉. 在线固相萃取-高效液相色谱-电感耦合等离子体质谱法同时测定血清中多溴二苯醚及其羟基代谢产物[J]. 分析化学, 2021, 49(4): 520-527. doi: 10.19756/j.issn.0253-3820.211074 shu

Citation: JIN Jin, SONG Shan-Jun, PENG Zi-Juan, GUO Feng, LI Peng-Hui. Determination of Polybrominated Diphenyl Ethers and Hydroxylated Analogues in Serum Using High Performance Liquid Chromatography-Inductively Coupled Plasma Mass Spectrometry with Online Solid Phase Extraction[J]. Chinese Journal of Analytical Chemistry, 2021, 49(4): 520-527. doi: 10.19756/j.issn.0253-3820.211074 shu

在线固相萃取-高效液相色谱-电感耦合等离子体质谱法同时测定血清中多溴二苯醚及其羟基代谢产物

金津 ^1,2, ,
宋善军 ^{2,
,} ,
彭子娟 ^2, ,
郭峰 ^{3,
,} ,
李彭辉 ^1,

1.
天津理工大学, 天津 300384;
2.
中国计量科学研究院, 北京 100029;
3.
国家地质实验测试中心, 北京 100037

通讯作者: 宋善军,E-mail:songsj@nim.ac.cn; 郭峰,E-mail:guofeng@mail.cgs.gov.cn

基金项目:
国家自然科学基金项目（Nos.21806158，21976044）资助。

摘要: 建立了在线固相萃取-高效液相色谱-电感耦合等离子体质谱法同时测定血清中6种多溴二苯醚和5种羟基代谢产物。200 μL血清样品经蛋白沉淀、稀释后，直接分析。采用自动进样，样品中的目标物在固相萃取柱上富集，甲醇-乙腈-水混合溶剂反向洗脱至液相色谱-电感耦合等离子体质谱仪完成分离分析。对上样速率、洗脱时间和洗脱溶剂等参数进行了优化，最终选择Oasis HLB型在线固相萃取柱，上样溶剂为纯水，上样速率为3.0 mL/min，洗脱溶剂为甲醇-乙腈-水（54：26：20，V/V），洗脱流速为1.0 mL/min，液相色谱柱为ZORBAX Eclipse Plus C₁₈。方法定量限为0.14~0.74 ng/L，基质加标回收率在61.8%~77.7%之间，检测结果的相对标准偏差在3.7%~10.1%（n=3）之间。将本方法应用于30个实际血清样品的分析检测，共检出4种多溴二苯醚和2种羟基多溴二苯醚，其赋存特征与已有报道一致。本方法可应用于大批量实际样品的分析检测，具有较强的实用价值。

关键词:

English

Determination of Polybrominated Diphenyl Ethers and Hydroxylated Analogues in Serum Using High Performance Liquid Chromatography-Inductively Coupled Plasma Mass Spectrometry with Online Solid Phase Extraction

JIN Jin ^1,2, ,
SONG Shan-Jun ^{2,
,} ,
PENG Zi-Juan ^2, ,
GUO Feng ^{3,
,} ,
LI Peng-Hui ^1,

1.
Tianjin University of Technology, Tianjin 300384, China;
2.
National Institute of Metrology, Beijing 100029, China;
3.
National Research Center for Geoanalysis, Beijing 100037, China

Corresponding author: SONG Shan-Jun, ; GUO Feng,

Received Date: 26 January 2021
Revised Date: 01 March 2021
Fund Project:
Supported by the National Natural Science Foundation of China (Nos.21806158, 21976044).

Abstract: Online solid phase extraction-high performance liquid chromatography-inductively coupled plasma mass spectrometry (Online SPE-HPLC-ICP-MS) technique was developed for simultaneous determination of six kinds of polybrominated diphenyl ethers and five kinds of hydroxyl metabolites in serum sample. By automatic injection, 200 μL of serum sample was directly analyzed after protein precipitation and dilution. The targets in samples were automatically enriched on a solid phase extraction column, and then separated and analyzed by liquid chromatography-inductively coupled plasma mass spectrometry with methanol/acetonitrile/water mixed solvent. After optimizing the main parameters such as loading rate, elution time and elution solvent, the Oasis HLB online solid phase extraction column was finally selected. The loading solvent was pure water with a rate of 3.0 mL/min, the elution solvent was the mixture of methanol, acetonitrile and water (54:26:20, V/V), the elution flow rate was 1.0 mL/min, and the liquid chromatography column was ZORBAX Eclipse Plus C₁₈. The limits of quantification (LOQ) of the method were 0.14-0.74 ng/L, the recoveries of matrix addition were from 61.8% to 77.7%, and the relative standard deviations (RSDs) of the results were from 3.7% to 10.1% (n=3). The established method was successfully applied to the analysis of 30 serum samples. Four kinds of polybrominated diphenyl ethers and two kinds of hydroxy polybrominated diphenyl ethers were detected, and their occurrence characteristics were consistent with the previous reports. The results showed that this method could be applied to analysis and detection of large quantities of actual samples, and had a great practical value.

Key words:

Online solid phase extraction
/ High performance liquid chromatography
/ Inductively coupled plasma mass spectrometry
/ Serum
/ Polybrominated diphenyl ethers
/ Hydroxy polybrominated diphenyl ethers

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沈阳化工大学材料科学与工程学院沈阳 110142

在线固相萃取-高效液相色谱-电感耦合等离子体质谱法同时测定血清中多溴二苯醚及其羟基代谢产物

通讯作者: 宋善军,E-mail:songsj@nim.ac.cn; 郭峰,E-mail:guofeng@mail.cgs.gov.cn

English

Determination of Polybrominated Diphenyl Ethers and Hydroxylated Analogues in Serum Using High Performance Liquid Chromatography-Inductively Coupled Plasma Mass Spectrometry with Online Solid Phase Extraction

Corresponding author: SONG Shan-Jun, ; GUO Feng,

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通讯作者: 陈斌, bchen63@163.com

中国化学会秘书处

在线固相萃取-高效液相色谱-电感耦合等离子体质谱法 同时测定血清中多溴二苯醚及其羟基代谢产物

通讯作者: 宋善军,E-mail:songsj@nim.ac.cn; 郭峰,E-mail:guofeng@mail.cgs.gov.cn

English

Determination of Polybrominated Diphenyl Ethers and Hydroxylated Analogues in Serum Using High Performance Liquid Chromatography-Inductively Coupled Plasma Mass Spectrometry with Online Solid Phase Extraction

Corresponding author: SONG Shan-Jun, ; GUO Feng,

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CCS Chemistry：颜徐州、鲍哲南： 你的皮肤可能是一片SPMs

CCS Chemistry：工作高效不疲劳，只须让催化剂动起来

CCS Chemistry：静电组装导向聚合- 聚电解质纳米凝胶量化制备新策略

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通讯作者: 陈斌, bchen63@163.com

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