PMID- 31078279
OWN - NLM
STAT- MEDLINE
DCOM- 20190724
LR  - 20191210
IS  - 1873-3778 (Electronic)
IS  - 0021-9673 (Linking)
VI  - 1601
DP  - 2019 Sep 13
TI  - Optimization and validation of a derivatization method with boron trifluoride in 
      ethanol for analysis of aromatic carboxylic acids in water.
PG  - 21-26
LID - S0021-9673(19)30495-9 [pii]
LID - 10.1016/j.chroma.2019.05.003 [doi]
AB  - Gas-chromatography (GC) analysis of carboxylic acids is limited by the high 
      polarity and low volatility of most of these compounds. Boron trifluoride (BF(3)) 
      mediated alkylation reactions is one of the most commonly used derivatization 
      methods for making carboxylic acids GC compatible. A semi-automated BF(3).EtOH 
      (ethanol) derivatization method was optimized for comprehensive two-dimensional 
      gas chromatography high-resolution mass spectrometry (GC x GC-HR MS) analysis of 
      carboxylic acids in solid phase extraction (SPE) extracts of oil polluted water. 
      The optimal derivatization method were found to be with addition of 300 muL 
      BF(3).EtOH per 200 muL sample and reaction at 75  degrees C for 24 h. Derivatives of eight 
      selected acids (aliphatic, mono- and di-aromatic) were stable over 12 h with 
      relative standard deviations (RSDs) of 2.0-10.7 %, the derivatization method was 
      repeatable (RSDs of 3.2-17.2 %), detection limits (DL) and limit of detections 
      (LODs) was in the range of DL = 0.53-1.63 ppb and LOD = 0.19-2.51 ppb for pure 
      acid standards, and DL = 0.18-3.41 ppb and LOD = 0.28-5.46 ppb for matrix matched 
      acid standards. Finally, the method was validated on the acidic fraction of a 
      mixed anion-exchange SPE of oil polluted water. Thousands of degradation products 
      from parent alkylated polycyclic aromatic hydrocarbons (PAHs) and aliphatic 
      hydrocarbons, such as aliphatic acids and mono-, di- and tri- aromatic acids were 
      analyzed by the applied method and compound groups were tentatively identified.
CI  - Copyright (c) 2019 Elsevier B.V. All rights reserved.
FAU - Kristensen, Mette
AU  - Kristensen M
AD  - Department of Plant and Environmental Sciences, University of Copenhagen, 
      Thorvaldsensvej 40, 1871, Frederiksberg C, Denmark. Electronic address: 
      mkri@plen.ku.dk.
FAU - Christensen, Peter
AU  - Christensen P
AD  - Department of Plant and Environmental Sciences, University of Copenhagen, 
      Thorvaldsensvej 40, 1871, Frederiksberg C, Denmark.
FAU - Christensen, Jan H
AU  - Christensen JH
AD  - Department of Plant and Environmental Sciences, University of Copenhagen, 
      Thorvaldsensvej 40, 1871, Frederiksberg C, Denmark.
LA  - eng
PT  - Journal Article
PT  - Validation Study
DEP - 20190504
PL  - Netherlands
TA  - J Chromatogr A
JT  - Journal of chromatography. A
JID - 9318488
RN  - 0 (Boranes)
RN  - 0 (Carboxylic Acids)
RN  - 0 (Petroleum)
RN  - 0 (Polycyclic Aromatic Hydrocarbons)
RN  - 0 (Water Pollutants, Chemical)
RN  - 059QF0KO0R (Water)
RN  - 3K9958V90M (Ethanol)
RN  - 7JGD48PX8P (boron trifluoride)
MH  - Alkylation
MH  - Boranes/*chemistry
MH  - Carboxylic Acids/*analysis
MH  - Environmental Monitoring/*methods
MH  - Ethanol/*chemistry
MH  - Gas Chromatography-Mass Spectrometry
MH  - Limit of Detection
MH  - Petroleum/analysis
MH  - Polycyclic Aromatic Hydrocarbons/analysis
MH  - Solid Phase Extraction
MH  - Water/*chemistry
MH  - Water Pollutants, Chemical/analysis
OTO - NOTNLM
OT  - Boron trifluoride-ethanol
OT  - Carboxylic acids
OT  - Crude oil
OT  - Derivatization
OT  - Gas chromatography
EDAT- 2019/05/13 06:00
MHDA- 2019/07/25 06:00
CRDT- 2019/05/13 06:00
PHST- 2019/02/11 00:00 [received]
PHST- 2019/04/30 00:00 [revised]
PHST- 2019/05/02 00:00 [accepted]
PHST- 2019/05/13 06:00 [pubmed]
PHST- 2019/07/25 06:00 [medline]
PHST- 2019/05/13 06:00 [entrez]
AID - S0021-9673(19)30495-9 [pii]
AID - 10.1016/j.chroma.2019.05.003 [doi]
PST - ppublish
SO  - J Chromatogr A. 2019 Sep 13;1601:21-26. doi: 10.1016/j.chroma.2019.05.003. Epub 
      2019 May 4.