PMID- 32505276
OWN - NLM
STAT- MEDLINE
DCOM- 20200805
LR  - 20200805
IS  - 1873-3778 (Electronic)
IS  - 0021-9673 (Linking)
VI  - 1623
DP  - 2020 Jul 19
TI  - Multiresidue analysis of 85 persistent organic pollutants in small human serum 
      samples by modified QuEChERS preparation with different ionization sources in 
      mass spectrometry.
PG  - 461170
LID - S0021-9673(20)30422-2 [pii]
LID - 10.1016/j.chroma.2020.461170 [doi]
AB  - In this study, a multiresidue analytical method was developed, validated, and 
      applied for quantifying 85 persistent organic pollutants (POPs), including 38 
      polychlorinated biphenyls (PCBs), 23 polybrominated diphenyl ethers (PBDEs), and 
      24 organochlorine pesticides (OCPs) from 200 muL of human serum. A modified 
      QuEChERS (Quick, Easy, Cheap, Effective, Rugged, and Safe) method was applied to 
      minimize the required sample amount and optimize various conditions including the 
      extraction solvent and the number of extractions. The extraction efficiency was 
      optimized using double extraction with an ethyl acetate/hexane/acetone mixture. 
      Gas chromatography coupled with triple-quadrupole mass spectrometry was used for 
      analysis, and two different ionization sources, electron impact ionization (EI) 
      and atmospheric pressure chemical ionization (APCI), were used to compare their 
      sensitivity. The APCI source employed soft ionization at atmospheric pressure, 
      producing abundant molecular ion formation with minimal fragmentation, in 
      contrast to extensive fragmentation caused by EI. Of the 85 POPs analyzed, 59 
      target compounds (69.4%) showed lower limits of detection that were two- to 
      fifty-fold lower in APCI than those determined using EI. The developed method was 
      validated for its detection limit (0.5-10 pg/mL for PCBs, 2-20 pg/mL for PBDEs, 
      and 2-40 pg/mL for OCPs), precision (0.8%-34.3% of coefficient of variation), 
      recovery (49.6%-77.1%), matrix effect (46.7%-156.9%), and accuracy (81.2%-113.1% 
      for PCBs, 85.8%-112.2% for PBDEs, and 55.2%-113.9% for OCPs). Its linearity was 
      R(2) > 0.99 for 84 compounds, and 96% average accuracy (for APCI) was obtained 
      using the National Institute of Standards and Technology (NIST) standard 
      reference materials (NIST 1957 and 1958). These ionization methods were compared 
      by analyzing 25 real human serum samples. The observed species were 1.1-24.6 
      pg/mL of 28 PCBs, 2.5 pg/mL of BDE-47, and 6.5-195.1 pg/mL of 6 organochlorine 
      pesticides (median concentration for each species), and only 11 compounds were 
      detected with APCI owing to its enhanced sensitivity.
CI  - Copyright (c) 2020 Elsevier B.V. All rights reserved.
FAU - Lee, Joo Eun
AU  - Lee JE
AD  - Doping Control Center, Korea Institute of Science and Technology, Hwarang-ro 
      14-gil 5, Seongbuk-gu, Seoul, 02792, Korea; Department of Chemistry, Sogang 
      University, Seoul, 04107, Korea.
FAU - Oh, Han Bin
AU  - Oh HB
AD  - Department of Chemistry, Sogang University, Seoul, 04107, Korea.
FAU - Im, Hosub
AU  - Im H
AD  - Institute for Life & Environmental Technology, Smartive Corporation, Dobong-ro 
      110na-gil, Dobong-gu, Seoul, 01454, Korea.
FAU - Han, Sang Beom
AU  - Han SB
AD  - Department of Pharmaceutical Analysis, College of Pharmacy, Chung-Ang University, 
      84 Heukseok-ro, Dongjak-gu, Seoul, 06974, Korea.
FAU - Kim, Ki Hun
AU  - Kim KH
AD  - Doping Control Center, Korea Institute of Science and Technology, Hwarang-ro 
      14-gil 5, Seongbuk-gu, Seoul, 02792, Korea. Electronic address: 
      kihun.kim@kist.re.kr.
LA  - eng
PT  - Journal Article
PT  - Validation Study
DEP - 20200512
PL  - Netherlands
TA  - J Chromatogr A
JT  - Journal of chromatography. A
JID - 9318488
RN  - 0 (Acetates)
RN  - 0 (Environmental Pollutants)
RN  - 0 (Halogenated Diphenyl Ethers)
RN  - 0 (Hexanes)
RN  - 0 (Hydrocarbons, Chlorinated)
RN  - 0 (Pesticides)
RN  - 0N97R5X10X (2,2',4,4'-tetrabromodiphenyl ether)
RN  - 1364PS73AF (Acetone)
RN  - 2DDG612ED8 (n-hexane)
RN  - 76845O8NMZ (ethyl acetate)
RN  - DFC2HB4I0K (Polychlorinated Biphenyls)
SB  - IM
MH  - Acetates/chemistry
MH  - Acetone/chemistry
MH  - Atmospheric Pressure
MH  - Environmental Pollutants/*blood/isolation & purification
MH  - Female
MH  - Gas Chromatography-Mass Spectrometry/*methods
MH  - Halogenated Diphenyl Ethers/blood
MH  - Hexanes/chemistry
MH  - Humans
MH  - Hydrocarbons, Chlorinated/blood
MH  - Limit of Detection
MH  - Pesticides/blood
MH  - Polychlorinated Biphenyls/blood
MH  - Tandem Mass Spectrometry/*methods
OTO - NOTNLM
OT  - Atmospheric pressure chemical ionization
OT  - Electron impact ionization
OT  - Human serum
OT  - Persistent organic pollutants
OT  - QuEChERS
COIS- Declaration of competing interest The authors declare that they have no known 
      competing financial interests or personal relationships that could have appeared 
      to influence the work reported in this paper.
EDAT- 2020/06/09 06:00
MHDA- 2020/08/06 06:00
CRDT- 2020/06/08 06:00
PHST- 2019/11/16 00:00 [received]
PHST- 2020/04/22 00:00 [revised]
PHST- 2020/04/23 00:00 [accepted]
PHST- 2020/06/08 06:00 [entrez]
PHST- 2020/06/09 06:00 [pubmed]
PHST- 2020/08/06 06:00 [medline]
AID - S0021-9673(20)30422-2 [pii]
AID - 10.1016/j.chroma.2020.461170 [doi]
PST - ppublish
SO  - J Chromatogr A. 2020 Jul 19;1623:461170. doi: 10.1016/j.chroma.2020.461170. Epub 
      2020 May 12.