PMID- 27614976
OWN - NLM
STAT- MEDLINE
DCOM- 20180119
LR  - 20180119
IS  - 1618-2650 (Electronic)
IS  - 1618-2642 (Linking)
VI  - 408
IP  - 27
DP  - 2016 Nov
TI  - Determination of novel brominated flame retardants and polybrominated diphenyl 
      ethers in serum using gas chromatography-mass spectrometry with two simplified 
      sample preparation procedures.
PG  - 7835-7844
AB  - 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 
      MgSO(4) and 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.
FAU - Gao, Le
AU  - Gao L
AD  - School of Public Health, Capital Medical University, Beijing, 100069, China.
AD  - Beijing Key Laboratory of Environmental Toxicology, Capital Medical University, 
      Beijing, 100069, China.
FAU - Li, Jian
AU  - Li J
AD  - School of Public Health, Capital Medical University, Beijing, 100069, China.
AD  - Beijing Key Laboratory of Environmental Toxicology, Capital Medical University, 
      Beijing, 100069, China.
FAU - Wu, Yandan
AU  - Wu Y
AD  - The Hospital of Shunyi District, Beijing, 101300, China.
FAU - Yu, Miaohao
AU  - Yu M
AD  - The Hospital of Shunyi District, Beijing, 101300, China.
FAU - Chen, Tian
AU  - Chen T
AD  - School of Public Health, Capital Medical University, Beijing, 100069, China.
AD  - Beijing Key Laboratory of Environmental Toxicology, Capital Medical University, 
      Beijing, 100069, China.
FAU - Shi, Zhixiong
AU  - Shi Z
AD  - School of Public Health, Capital Medical University, Beijing, 100069, China. 
      szx0127@ccmu.edu.cn.
AD  - Beijing Key Laboratory of Environmental Toxicology, Capital Medical University, 
      Beijing, 100069, China. szx0127@ccmu.edu.cn.
FAU - Zhou, Xianqing
AU  - Zhou X
AD  - School of Public Health, Capital Medical University, Beijing, 100069, China.
AD  - Beijing Key Laboratory of Environmental Toxicology, Capital Medical University, 
      Beijing, 100069, China.
FAU - Sun, Zhiwei
AU  - Sun Z
AD  - School of Public Health, Capital Medical University, Beijing, 100069, China.
AD  - Beijing Key Laboratory of Environmental Toxicology, Capital Medical University, 
      Beijing, 100069, China.
LA  - eng
PT  - Journal Article
DEP - 20160910
PL  - Germany
TA  - Anal Bioanal Chem
JT  - Analytical and bioanalytical chemistry
JID - 101134327
RN  - 0 (Flame Retardants)
RN  - 0 (Halogenated Diphenyl Ethers)
RN  - 0 (Hexanes)
RN  - 0 (Sulfuric Acids)
RN  - 1364PS73AF (Acetone)
RN  - 588X2YUY0A (Methylene Chloride)
RN  - ND2M416302 (2-Propanol)
RN  - O40UQP6WCF (sulfuric acid)
RN  - Y4S76JWI15 (Methanol)
SB  - IM
MH  - 2-Propanol/chemistry
MH  - Acetone/chemistry
MH  - Flame Retardants/*analysis
MH  - Gas Chromatography-Mass Spectrometry/*methods
MH  - Halogenated Diphenyl Ethers/*blood
MH  - Hexanes/chemistry
MH  - Humans
MH  - Limit of Detection
MH  - Male
MH  - Methanol/chemistry
MH  - Methylene Chloride/chemistry
MH  - Reproducibility of Results
MH  - Solid Phase Extraction/*methods
MH  - Sulfuric Acids/chemistry
OTO - NOTNLM
OT  - Gas chromatography-mass spectrometry
OT  - Novel brominated flame retardants
OT  - Polybrominated diphenyl ethers
OT  - QuEChERS
OT  - Serum
EDAT- 2016/09/12 06:00
MHDA- 2018/01/20 06:00
CRDT- 2016/09/12 06:00
PHST- 2016/04/30 00:00 [received]
PHST- 2016/08/16 00:00 [accepted]
PHST- 2016/07/28 00:00 [revised]
PHST- 2016/09/12 06:00 [pubmed]
PHST- 2018/01/20 06:00 [medline]
PHST- 2016/09/12 06:00 [entrez]
AID - 10.1007/s00216-016-9887-z [pii]
AID - 10.1007/s00216-016-9887-z [doi]
PST - ppublish
SO  - Anal Bioanal Chem. 2016 Nov;408(27):7835-7844. doi: 10.1007/s00216-016-9887-z. 
      Epub 2016 Sep 10.