Determination of Decabromodiphenyl Ether and Decabromodiphenyl Ethane in Sediments by High-Performance Liquid Chromatography Coupled with Inductively Coupled Plasma-Mass Spectrometry
10.19756/j.issn.0253-3820.251065
- VernacularTitle:高效液相色谱-电感耦合等离子体质谱联用技术测定沉积物中十溴二苯醚和十溴二苯乙烷
- Author:
Xiao-Fei WEI
1
;
Jing WU
;
Zhuo HAN
;
Yu-Zhu ZHANG
;
Zi-Juan PENG
;
Peng-Hui LI
;
Shan-Jun SONG
Author Information
1. 天津理工大学环境科学与安全工程学院,天津 300382;中国计量科学研究院,北京 100029
- Keywords:
High-performance liquid chromatography-inductively coupled plasma mass spectrometry;
Sediment;
Decabromodiphenyl ether;
Decabromodiphenyl ethane
- From:
Chinese Journal of Analytical Chemistry
2025;53(9):1526-1535
- CountryChina
- Language:Chinese
-
Abstract:
Decabromodiphenyl ether(BDE-209)and decabromodiphenyl ethane(DBDPE)are widely used brominated flame retardants,which have been detected in the atmosphere,water,soil,and various organisms.In this study,a method based on high-performance liquid chromatography-inductively coupled plasma-mass spectrometry(HPLC-ICP-MS)was developed for determination of BDE-209 and DBDPE in sediment.Firstly,the target compounds in the sediments were extracted by accelerated solvent extraction(ASE),and the extraction solvent was hexane/dichloromethane(1∶1,V/V).The extract was concentrated by rotary evaporation and purified by a composite silica gel column(6 g neutral silica gel,8 g acidic silica gel,and 4 g anhydrous sodium sulfate),concentrated by nitrogen blowing,and then re-dissolved with 1 mL of toluene for instrumental determination.The chromatographic separation was carried out on a TC-C18(2)column(250 mm×4.6 mm)with isocratic elution using methanol-isopropanol-water(89∶6∶5,V/V)as the mobile phase,and the samples were separated within 20 min.Further,the Br element was quantified by ICP-MS to realize the detection of the target.The results showed that the method established in this study exhibited good linearity(R2>0.999)in the range of 100-10000 ng/mL,and the limits of quantification(LOQs)of the method were 2.0 ng/g for BDE-209 and 10.0 ng/g for DBDPE,with the relative standard deviations(RSDs,n=3)lower than 10%,and the recoveries were in the acceptable range(80.9%-120.7%).The matrix effect was effectively controlled within 10%.In addition,by analyzing the actual sediment samples from Guangxi,a background point,and Taizhou,Zhejiang,a typical contaminated area,it was found that neither BDE-209 nor DBDPE was detected in the sediment from Guangxi,while the concentrations of BDE-209 and DBDPE in the sediment from Zhejiang ranged from 1591.8 to 3362.9 ng/g,which further demonstrated the applicability and reliability of the method for analyzing actual environmental samples.This study provided a strong technical support for the accurate detection of POPs in the environment.
