PMID- 32317103
OWN - NLM
STAT- MEDLINE
DCOM- 20200722
LR  - 20200722
IS  - 1873-3778 (Electronic)
IS  - 0021-9673 (Linking)
VI  - 1621
DP  - 2020 Jun 21
TI  - Optimization of a solid-phase microextraction technique for chloro‑ and nitro- 
      substituted aromatic compounds using design of experiments.
PG  - 461083
LID - S0021-9673(20)30304-6 [pii]
LID - 10.1016/j.chroma.2020.461083 [doi]
AB  - A rapid and sensitive direct immersion solid-phase microextraction (SPME) 
      technique for the analysis of seven chloro (Cl-) and nitro (NO(2)-) substituted 
      anilines, toluenes, and nitrobenzenes from small volume (1.5 mL) aqueous samples 
      was optimized for gas chromatography using Design of Experiments (DoE). Screening 
      of the SPME factors was performed by a fractional factorial DoE, and the 
      optimization of influential factors was achieved with a central composite 
      multi-response surface DoE. Extraction time, pre-SPME agitation speed, extraction 
      temperature, and desorption temperature were identified as significant factors 
      and their values were set using a desirability function that maximized the 
      extraction of the seven target analytes. Extraction time and agitation speed 
      showed significant interactions for most analytes (alpha = 0.05). The relative 
      standard deviations (RSDs) for within-day and between-day analyses were below 8%, 
      suggesting that the method was repeatable and reproducible. The obtained limits 
      of detection were in the low mug/L range (1-10) using a Flame Ionization Detector, 
      far below what is needed for industrial contaminated sites (usually >1 mg/L). The 
      optimized SPME method increased the analyte concentration up to 2-3 orders of 
      magnitude compared with direct GC injection. The optimized SPME method was 
      applied to two groundwater samples from a contaminated site in which the 
      concentrations of three of the target analytes were ranged from 0.06 to 9.42 mg/L 
      with RSDs <11%. When the concentrations of the target analytes in the sample 
      matrix were higher than 0.5 mg/L, a competition for the SPME extraction sites was 
      observed where analytes with higher affinity for the fiber material replaced the 
      analytes with lower affinity. As a result, dilution of highly contaminated 
      samples is recommended. This study provided for the first time an analytical 
      method for the quantification of frequently co-occurring contaminants from the 
      chloro‑ and nitro- substituted aniline, toluene, and nitrobenzene families.
CI  - Copyright (c) 2020 Elsevier B.V. All rights reserved.
FAU - Suchana, Shamsunnahar
AU  - Suchana S
AD  - Department of Civil and Mineral Engineering, University of Toronto, 35 St George 
      Street, M5S 1A4 Toronto, ON, Canada.
FAU - Passeport, Elodie
AU  - Passeport E
AD  - Department of Civil and Mineral Engineering, University of Toronto, 35 St George 
      Street, M5S 1A4 Toronto, ON, Canada; Department of Chemical Engineering and 
      Applied Chemistry, University of Toronto, 200 College Street, M5S 3E5 Toronto, 
      ON, Canada. Electronic address: elodie.passeport@utoronto.ca.
LA  - eng
PT  - Journal Article
DEP - 20200415
PL  - Netherlands
TA  - J Chromatogr A
JT  - Journal of chromatography. A
JID - 9318488
RN  - 0 (Hydrocarbons, Aromatic)
RN  - 0 (Nitro Compounds)
RN  - 0 (Salts)
RN  - 0 (Water Pollutants, Chemical)
SB  - IM
MH  - Analysis of Variance
MH  - Calibration
MH  - Groundwater/chemistry
MH  - Hydrocarbons, Aromatic/*analysis
MH  - Limit of Detection
MH  - Models, Theoretical
MH  - Nitro Compounds/*analysis
MH  - Reproducibility of Results
MH  - Salts/chemistry
MH  - Solid Phase Microextraction/*methods
MH  - Temperature
MH  - Time Factors
MH  - Water Pollutants, Chemical/analysis
OTO - NOTNLM
OT  - Competitive sorption
OT  - Design of experiments
OT  - Gas chromatography
OT  - Response surface design
OT  - Solid-phase microextraction
OT  - Substituted aromatic compounds
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- 2020/04/23 06:00
MHDA- 2020/07/23 06:00
CRDT- 2020/04/23 06:00
PHST- 2019/09/21 00:00 [received]
PHST- 2020/03/24 00:00 [revised]
PHST- 2020/03/25 00:00 [accepted]
PHST- 2020/04/23 06:00 [pubmed]
PHST- 2020/07/23 06:00 [medline]
PHST- 2020/04/23 06:00 [entrez]
AID - S0021-9673(20)30304-6 [pii]
AID - 10.1016/j.chroma.2020.461083 [doi]
PST - ppublish
SO  - J Chromatogr A. 2020 Jun 21;1621:461083. doi: 10.1016/j.chroma.2020.461083. Epub 
      2020 Apr 15.