多种色谱质谱联用技术测定沉积物中的十溴二苯醚  

Determination of decabromodiphenyl ether in sediment using chromatography-mass spectrometry methods

作　　者：王惠宇 宋善军 邵明武[2] 尹建道[1] 杨晨[1] 李彭辉[1] WANG Huiyu;SONG Shanjun;SHAO Mingwu;YIN Jiandao;YANG Chen;LI Penghui(Tianjin University of Technology,Tianjin,300384,China;National Institute of Metrology,China,Beijing,100029,China)

机构地区：[1]天津理工大学,天津300384 [2]中国计量科学研究院,北京100029

出　　处：《环境化学》2019年第10期2203-2211,共9页Environmental Chemistry

基　　金：国家质量基础项目(2016YFF0201102);国家自然科学基金青年基金(41601548)资助~~

摘　　要：随着十溴二苯醚(BDE-209)正式进入《斯德哥尔摩公约》名单,准确测量其浓度水平对研究其环境行为具有重要意义.本文对多种色谱质谱联用技术——气相色谱-负化学电离质谱(GC-NCI-MS)、气相色谱-电子轰击电离质谱(GC-EI-MS)、气相色谱-电感耦合等离子体质谱(GC-ICP-MS)和高效液相色谱-电感耦合等离子体质谱(HPLC-ICP-MS)进行了优化和评估,并对其在实际环境沉积物样品中检测BDE-209的性能进行了考察.4种检测方法的定量限为3—200 ng·mL^-1,在0.5-10μg·mL^-1的范围内有良好的线性关系(r^2>0.995),测量结果的相对标准偏差(RSD)在0.5%—8.7%之间,可以满足BDE-209分析检测的需求.应用到沉积物实际样品的检测时,各方法测量结果的RSD为0.7%—15.7%,基质效应为98%—166%,其中GC-EI-MS和GC-NCI-MS表现出基质增强效应且分析结果的稳定性受到影响,可通过内标或基质加标方式进行校正,GC-ICP-MS、HPLC-ICP-MS几乎不受实际样品基质的影响,测量结果的准确性良好.The accurate determination of decabrominated diphenyl ethers(BDE-209)is important for the study of its environmental behavior,especially after BDE-209 was officially listed in Stockholm Convention in 2017.This research optimized and evaluated most widely used gas/liquid chromatography-mass spectrometry methods for BDE-209 determination,including GC-NCI-MS,GC-EI-MS,GC-ICP-MS and HPLC-ICP-MS.The performances of each method were investigated for standard solution determination and field sediment samples determination.The limits of quantification ranged from 3—200 ng·mL^-1 and linear fitting with coefficients>0.995 ranging from 0.5 to 10μg·mL^-1.The precision of each method was illustrated by relative standard deviation(RSD) of analysis results(n=5) ranging from 0.5%—8.7%.The performances of each method on field sediment sample analysis were investigated and the results showed the precision and matrix effects were 0.7%—15.7%and 98%—166%.GC-EI-MS and GC-NCI-MS signal intensities were enhanced,and the precision was affected by introduction of sediment matrix.Internal standards and matrix match calibration were suggested for these methods to analyze field samples.GC-ICP-MS and HPLC-ICP-MS showed robust performances with neglectable effects by sample matrix.

关 键 词：十溴二苯醚 沉积物 色谱质谱技术 方法性能 基质效应 

分 类 号：R28[医药卫生—中药学]