PMID- 24484690
OWN - NLM
STAT- MEDLINE
DCOM- 20140722
LR  - 20191210
IS  - 1873-3778 (Electronic)
IS  - 0021-9673 (Linking)
VI  - 1330
DP  - 2014 Feb 21
TI  - New perspectives on diastereoselective determination of hexabromocyclododecane 
      traces in fish by ultra high performance liquid chromatography-high resolution 
      orbitrap mass spectrometry.
PG  - 30-9
LID - S0021-9673(14)00085-5 [pii]
LID - 10.1016/j.chroma.2014.01.023 [doi]
AB  - A new analytical method is presented for diastereoisomer-specific identification 
      and quantitation of hexabromocyclododecanes (HBCD) in fish samples. The method is 
      based on extraction of the target analytes from samples with a mixture of organic 
      solvents, with further three-stage clean-up including destructive removal of 
      matrix components with sulphuric acid and acid-impregnated silica gel, and 
      Florisil adsorption column chromatography. Ultra high performance liquid 
      chromatography (UPLC) coupled with high resolution (HR) Orbitrap mass 
      spectrometry featuring heated electrospray ionization (HESI-II) interface 
      operated in negative ion mode was employed for the identification/quantitation of 
      contaminants. The developed methodology was robustly validated in terms of 
      recovery, repeatability, intermediate precision, linear calibration ranges, 
      limits of detection and quantitation, and used for analysis of twenty five Baltic 
      wild salmon (Salmo salar) samples. Under the optimized conditions, recoveries for 
      selected analytes were within the range of 91.4-103.6%, and the repeatability and 
      intermediate precision in terms of relative standard deviations (RSDs) were in 
      the ranges 1.6-8.3% and 1.6-12.5%, respectively, for all three validation levels. 
      The elaborated method achieved instrumental limits of quantification (i-LOQ) of 
      1.3-3.0pg on column for three HBCD diastereoisomers corresponding to the method 
      LOQ of 0.005-0.012ngg(-1) wet weight (w.w.) The presence of HBCD diastereoisomers 
      was confirmed in all the analyzed Baltic salmon samples in the concentration 
      range of 0.39-3.82ngg(-1) w.w. with an average of 1.59ngg(-1) w.w. for total 
      HBCD. The diastereomer pattern typical for aquatic biota was observed with strong 
      predominance of alpha-HBCD. The newly developed methodology could be employed for a 
      regular diastereomer-specific monitoring of HBCD content in fish samples, 
      representing a good alternative to existing LC-MS/MS methods in terms of 
      sensitivity and accuracy, and providing further possibilities for inclusion of 
      other contaminants in the scope of analysis.
CI  - Copyright (c) 2014 Elsevier B.V. All rights reserved.
FAU - Zacs, D
AU  - Zacs D
AD  - Institute of Food Safety, Animal Health and Environment "BIOR", Lejupes iela 3, 
      Riga LV-1076, Latvia; University of Latvia, Department of Chemistry, Kr. 
      Valdemara iela 48, Riga LV-1013, Latvia. Electronic address: 
      dzintars.zachs@gmail.com.
FAU - Rjabova, J
AU  - Rjabova J
AD  - Institute of Food Safety, Animal Health and Environment "BIOR", Lejupes iela 3, 
      Riga LV-1076, Latvia.
FAU - Bartkevics, V
AU  - Bartkevics V
AD  - Institute of Food Safety, Animal Health and Environment "BIOR", Lejupes iela 3, 
      Riga LV-1076, Latvia; University of Latvia, Department of Chemistry, Kr. 
      Valdemara iela 48, Riga LV-1013, Latvia.
LA  - eng
PT  - Journal Article
PT  - Research Support, Non-U.S. Gov't
PT  - Validation Study
DEP - 20140118
PL  - Netherlands
TA  - J Chromatogr A
JT  - Journal of chromatography. A
JID - 9318488
RN  - 0 (Flame Retardants)
RN  - 0 (Hydrocarbons, Brominated)
RN  - 0 (Water Pollutants, Chemical)
RN  - 5I9835JO3M (hexabromocyclododecane)
RN  - 60650-90-0 (Silica Gel)
SB  - IM
MH  - Animals
MH  - Calibration
MH  - Chromatography, High Pressure Liquid/methods
MH  - Flame Retardants/*analysis
MH  - Hydrocarbons, Brominated/*analysis
MH  - *Salmo salar
MH  - Silica Gel
MH  - Spectrometry, Mass, Electrospray Ionization/methods
MH  - Stereoisomerism
MH  - Water Pollutants, Chemical/*analysis
OTO - NOTNLM
OT  - BFRs
OT  - Fish
OT  - Hexabromocyclododecane
OT  - Orbitrap-HRMS
OT  - UPLC
EDAT- 2014/02/04 06:00
MHDA- 2014/07/23 06:00
CRDT- 2014/02/04 06:00
PHST- 2013/11/11 00:00 [received]
PHST- 2013/12/23 00:00 [revised]
PHST- 2014/01/08 00:00 [accepted]
PHST- 2014/02/04 06:00 [entrez]
PHST- 2014/02/04 06:00 [pubmed]
PHST- 2014/07/23 06:00 [medline]
AID - S0021-9673(14)00085-5 [pii]
AID - 10.1016/j.chroma.2014.01.023 [doi]
PST - ppublish
SO  - J Chromatogr A. 2014 Feb 21;1330:30-9. doi: 10.1016/j.chroma.2014.01.023. Epub 
      2014 Jan 18.