PMID- 28415017
OWN - NLM
STAT- MEDLINE
DCOM- 20170531
LR  - 20191210
IS  - 1873-376X (Electronic)
IS  - 1570-0232 (Linking)
VI  - 1053
DP  - 2017 May 15
TI  - Accelerated solvent extraction method for the quantification of polycyclic 
      aromatic hydrocarbons in cocoa beans by gas chromatography-mass spectrometry.
PG  - 87-100
LID - S1570-0232(16)31043-1 [pii]
LID - 10.1016/j.jchromb.2017.03.017 [doi]
AB  - An accelerated solvent extraction (ASE) procedure for use with gas 
      chromatography-mass spectrometry (GC-MS) was optimized for the determination of 
      eight polycyclic aromatic hydrocarbons (PAHs) in cocoa beans. Plackett-Burman and 
      rotatable central composite design (RCCD) indicated that three variables affected 
      the recoveries of PAHs during the extraction and purification steps: agitation 
      time in the second liquid-liquid partition, weight of silica gel in the column, 
      and volume of hexane for PAH elution from the column. After obtaining the optimal 
      conditions, a single laboratory method validation was performed. Linearity was 
      demonstrated for benzo[a]pyrene in the concentration range from 0.5 to 
      8.0mgkg(-1) of sample, corresponding to 1.25-20.0mugkg(-1) of cocoa on a fat 
      basis. For the other analytes, linearity was observed from 0.75 to 8.0mugkg(-1) of 
      sample (1.88-20.0mugkg(-1) of cocoa on a fat basis). Significant matrix effects 
      were found for chrysene and benzo[b]fluoranthene. The precision of the method was 
      verified with relative standard deviations (RSDs) ranging from 2.57 to 14.13% and 
      from 4.36 to 19.77% under repeatability and intermediate precision conditions, 
      respectively. The average recoveries of the eight PAHs ranged from 74.99 to 
      109.73%. These parameters, limits and measurement uncertainties met the 
      performance criteria established by European Union regulations, except for the 
      theoretical limit of detection for chrysene. The method was applied to the 
      analysis of samples of Brazilian cocoa beans, and only one sample was found to 
      have a PAH content above the maximum limit defined by the European Union 
      legislation. This optimized and validated method is intended to be used as part 
      of the official Brazilian monitoring programs investigating contaminants and 
      residues in food.
CI  - Copyright (c) 2017 Elsevier B.V. All rights reserved.
FAU - Belo, Renata Franca Cassimiro
AU  - Belo RFC
AD  - Federal University of Minas Gerais (UFMG), Faculty of Pharmacy (FAFAR), 
      Department of Food Science, Av. Antonio Carlos, 6627, Campus da UFMG, Pampulha, 
      31270-010, Belo Horizonte, MG, Brazil.
FAU - Figueiredo, Julia Pereira
AU  - Figueiredo JP
AD  - Ministry of Agriculture, Livestock and Food Supply (MAPA), National Laboratory of 
      Minas Gerais (LANAGRO-MG), Av. Romulo Joviano s/n, Centro, 33.600-000, Pedro 
      Leopoldo, MG, Brazil.
FAU - Nunes, Carolina Mariana
AU  - Nunes CM
AD  - Ministry of Agriculture, Livestock and Food Supply (MAPA), National Laboratory of 
      Minas Gerais (LANAGRO-MG), Av. Romulo Joviano s/n, Centro, 33.600-000, Pedro 
      Leopoldo, MG, Brazil.
FAU - Pissinatti, Rafael
AU  - Pissinatti R
AD  - Ministry of Agriculture, Livestock and Food Supply (MAPA), National Laboratory of 
      Minas Gerais (LANAGRO-MG), Av. Romulo Joviano s/n, Centro, 33.600-000, Pedro 
      Leopoldo, MG, Brazil.
FAU - Souza, Scheilla Vitorino Carvalho de
AU  - Souza SVC
AD  - Federal University of Minas Gerais (UFMG), Faculty of Pharmacy (FAFAR), 
      Department of Food Science, Av. Antonio Carlos, 6627, Campus da UFMG, Pampulha, 
      31270-010, Belo Horizonte, MG, Brazil.
FAU - Junqueira, Roberto Goncalves
AU  - Junqueira RG
AD  - Federal University of Minas Gerais (UFMG), Faculty of Pharmacy (FAFAR), 
      Department of Food Science, Av. Antonio Carlos, 6627, Campus da UFMG, Pampulha, 
      31270-010, Belo Horizonte, MG, Brazil. Electronic address: rjunqueira@ufmg.br.
LA  - eng
PT  - Journal Article
PT  - Validation Study
DEP - 20170330
PL  - Netherlands
TA  - J Chromatogr B Analyt Technol Biomed Life Sci
JT  - Journal of chromatography. B, Analytical technologies in the biomedical and life 
      sciences
JID - 101139554
RN  - 0 (Environmental Pollutants)
RN  - 0 (Polycyclic Aromatic Hydrocarbons)
SB  - IM
MH  - Cacao/*chemistry
MH  - Environmental Pollutants/*analysis
MH  - Food Contamination/*analysis
MH  - Gas Chromatography-Mass Spectrometry/*methods
MH  - Limit of Detection
MH  - Polycyclic Aromatic Hydrocarbons/*analysis
MH  - Seeds/*chemistry
OTO - NOTNLM
OT  - Accelerated solvent extraction
OT  - Cocoa bean
OT  - Gas chromatography
OT  - Mass spectrometry
OT  - Polycyclic aromatic hydrocarbons
OT  - Single laboratory method validation
EDAT- 2017/04/18 06:00
MHDA- 2017/06/01 06:00
CRDT- 2017/04/18 06:00
PHST- 2016/11/02 00:00 [received]
PHST- 2017/01/16 00:00 [revised]
PHST- 2017/03/18 00:00 [accepted]
PHST- 2017/04/18 06:00 [pubmed]
PHST- 2017/06/01 06:00 [medline]
PHST- 2017/04/18 06:00 [entrez]
AID - S1570-0232(16)31043-1 [pii]
AID - 10.1016/j.jchromb.2017.03.017 [doi]
PST - ppublish
SO  - J Chromatogr B Analyt Technol Biomed Life Sci. 2017 May 15;1053:87-100. doi: 
      10.1016/j.jchromb.2017.03.017. Epub 2017 Mar 30.