干旱区生态环境知识资源中心(Arid): 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

Arid

	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
其他题名	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
	金津; 宋善军; 彭子娟; 郭峰; 李彭辉
来源期刊	分析化学
ISSN	0253-3820
出版年	2021
卷号	49 期号:4 页码:0253-3820
中文摘要	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 muL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 C_(18)。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。
英文摘要	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 muL 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 C_(18). 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.
中文关键词	在线固相萃取 ; 高效液相色谱 ; 电感耦合等离子体质谱 ; 血清 ; 多溴二苯醚 ; 羟基多溴二苯醚
英文关键词	Online solid phase extraction High performance liquid chromatography Inductively coupled plasma mass spectrometry Serum Polybrominated diphenyl ethers Hydroxy polybrominated diphenyl ethers
类型	Article
语种	中文
国家	中国
收录类别	CSCD
WOS类目	Chemistry
CSCD记录号	CSCD:6948664
资源类型	期刊论文
条目标识符	http://119.78.100.177/qdio/handle/2XILL650/354235
作者单位	金津, 天津理工大学;;中国计量科学研究院, ;;, ;;, 天津;;北京 300384;;100029, 中国.; 宋善军, 中国计量科学研究院, 北京 100029, 中国.; 彭子娟, 中国计量科学研究院, 北京 100029, 中国.; 郭峰, 国家地质实验测试中心, 北京 100037, 中国.; 李彭辉, 天津理工大学, 天津 300384, 中国.
推荐引用方式 GB/T 7714	金津,宋善军,彭子娟,等. 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],2021,49(4):0253-3820.
APA	金津,宋善军,彭子娟,郭峰,&李彭辉.(2021).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.分析化学,49(4),0253-3820.
MLA	金津,et al."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".分析化学 49.4(2021):0253-3820.