Determination of novel brominated flame retardants and polybrominated diphenyl ethers in serum using gas chromatography-mass spectrometry with two simplified sample preparation procedures.
Two simple and efficient pretreatment procedures have been developed for the simultaneous extraction and cleanup of six novel brominated flame retardants (NBFRs) and eight common polybrominated diphenyl ethers (PBDEs) in human serum. The first sample pretreatment procedure was a quick, easy, cheap, effective, rugged, and safe (QuEChERS)-based approach. An acetone/hexane mixture was employed to isolate the lipid and analytes from the serum with a combination of MgSO4and NaCl, followed by a dispersive solid-phase extraction (d-SPE) step using C18 particles as a sorbent. The second sample pretreatment procedure was based on solid-phase extraction. The sample extraction and cleanup were conducted directly on an Oasis HLB SPE column using 5 % aqueous isopropanol, concentrated sulfuric acid, and 10 % aqueous methanol, followed by elution with dichloromethane. The NBFRs and PBDEs were then detected using gas chromatography-negative chemical ionization mass spectrometry (GC-NCI MS). The methods were assessed for repeatability, accuracy, selectivity, limits of detection (LODs), and linearity. The results of spike recovery experiments in fetal bovine serum showed that average recoveries ranged from 77.9 % to 128.8 % with relative standard deviations (RSDs) from 0.73 % to 12.37 % for most of the analytes. The LODs for the analytes in fetal bovine serum ranged from 0.3 to 50.8 pg/mL except for decabromodiphenyl ethane. The proposed method was successfully applied to the determination of the 14 brominated flame retardants in human serum. The two pretreatment procedures described here are simple, accurate, and precise, and are suitable for the routine analysis of human serum. Graphical Abstract Workflow of a QuEChERS-based approach (top) and an SPE-based approach (bottom) for the detection of PBDEs and NBFRs in serum.
School of Public Health, Capital Medical University, Beijing, 100069, China.|Beijing Key Laboratory of Environmental Toxicology, Capital Medical University, Beijing, 100069, China.
Le
L
Gao
School of Public Health, Capital Medical University, Beijing, 100069, China.|Beijing Key Laboratory of Environmental Toxicology, Capital Medical University, Beijing, 100069, China.
Jian
J
Li
The Hospital of Shunyi District, Beijing, 101300, China.
Yandan
Y
Wu
The Hospital of Shunyi District, Beijing, 101300, China.
Miaohao
M
Yu
School of Public Health, Capital Medical University, Beijing, 100069, China.|Beijing Key Laboratory of Environmental Toxicology, Capital Medical University, Beijing, 100069, China.
Tian
T
Chen
School of Public Health, Capital Medical University, Beijing, 100069, China. szx0127@ccmu.edu.cn.|Beijing Key Laboratory of Environmental Toxicology, Capital Medical University, Beijing, 100069, China. szx0127@ccmu.edu.cn.
Zhixiong
Z
Shi
School of Public Health, Capital Medical University, Beijing, 100069, China.|Beijing Key Laboratory of Environmental Toxicology, Capital Medical University, Beijing, 100069, China.
Xianqing
X
Zhou
School of Public Health, Capital Medical University, Beijing, 100069, China.|Beijing Key Laboratory of Environmental Toxicology, Capital Medical University, Beijing, 100069, China.
Zhiwei
Z
Sun
D019840:2-Propanol / Q000737:chemistry; D000096:Acetone / Q000737:chemistry; D005411:Flame Retardants / Q000032:analysis*; D008401:Gas Chromatography-Mass Spectrometry / Q000379:methods*; D055768:Halogenated Diphenyl Ethers / Q000097:blood*; D006586:Hexanes / Q000737:chemistry; D006801:Humans; D057230:Limit of Detection; D008297:Male; D000432:Methanol / Q000737:chemistry; D008752:Methylene Chloride / Q000737:chemistry; D015203:Reproducibility of Results; D052616:Solid Phase Extraction / Q000379:methods*; D013464:Sulfuric Acids / Q000737:chemistry
D005411:Flame Retardants; D055768:Halogenated Diphenyl Ethers; D006586:Hexanes; D013464:Sulfuric Acids; D000096:Acetone; D008752:Methylene Chloride; D019840:2-Propanol; C033158:sulfuric acid; D000432:Methanol
Gas chromatography–mass spectrometry; Novel brominated flame retardants; Polybrominated diphenyl ethers; QuEChERS; Serum