PMID- 19292459
OWN - NLM
STAT- MEDLINE
DCOM- 20090506
LR  - 20090318
IS  - 1520-5118 (Electronic)
IS  - 0021-8561 (Linking)
VI  - 57
IP  - 6
DP  - 2009 Mar 25
TI  - Development of an analytical scheme for the determination of pyrethroid 
      pesticides in composite diet samples.
PG  - 2096-104
LID - 10.1021/jf8032446 [doi]
AB  - Analysis of an individual's total daily food intake may be used to determine 
      aggregate dietary ingestion of given compounds. However, the resulting composite 
      sample represents a complex mixture, and measurement of such can often prove to 
      be difficult. In this work, an analytical scheme was developed for the 
      determination of 12 select pyrethroid pesticides in dietary samples. In the first 
      phase of the study, several cleanup steps were investigated for their 
      effectiveness in removing interferences in samples with a range of fat content 
      (1-10%). Food samples were homogenized in the laboratory, and preparatory 
      techniques were evaluated through recoveries from fortified samples. The selected 
      final procedure consisted of a lyophilization step prior to sample extraction. A 
      sequential 2-fold cleanup procedure of the extract included diatomaceous earth 
      for removal of lipid components followed with a combination of deactivated 
      alumina and C(18) for the simultaneous removal of polar and nonpolar 
      interferences. Recoveries from fortified composite diet samples (10 microg 
      kg(-1)) ranged from 50.2 to 147%. In the second phase of this work, three 
      instrumental techniques [gas chromatography-microelectron capture detection 
      (GC-microECD), GC-quadrupole mass spectrometry (GC-quadrupole-MS), and GC-ion 
      trap-MS/MS] were compared for greatest sensitivity. GC-quadrupole-MS operated in 
      selective ion monitoring (SIM) mode proved to be most sensitive, yielding method 
      detection limits of approximately 1 microg kg(-1). The developed 
      extraction/instrumental scheme was applied to samples collected in an exposure 
      measurement field study. The samples were fortified and analyte recoveries were 
      acceptable (75.9-125%); however, compounds coextracted from the food matrix 
      prevented quantitation of four of the pyrethroid analytes in two of the samples 
      considered.
FAU - Vonderheide, Anne P
AU  - Vonderheide AP
AD  - National Exposure Research Laboratory, Microbiological and Chemical Exposure 
      Assessment Research Division, Chemical Exposure Research Branch, and National 
      Council on the Aging, US Environmental Protection Agency, Cincinnati, Ohio 45268, 
      USA.
FAU - Kauffman, Peter E
AU  - Kauffman PE
FAU - Hieber, Thomas E
AU  - Hieber TE
FAU - Brisbin, Judith A
AU  - Brisbin JA
FAU - Melnyk, Lisa Jo
AU  - Melnyk LJ
FAU - Morgan, Jeffrey N
AU  - Morgan JN
LA  - eng
PT  - Journal Article
PT  - Research Support, U.S. Gov't, Non-P.H.S.
PL  - United States
TA  - J Agric Food Chem
JT  - Journal of agricultural and food chemistry
JID - 0374755
RN  - 0 (Dietary Fats)
RN  - 0 (Insecticides)
RN  - 0 (Pyrethrins)
SB  - IM
MH  - Chromatography, Gas/methods
MH  - Dietary Fats/analysis
MH  - Food Analysis/*methods
MH  - Food Contamination/*analysis
MH  - Freeze Drying
MH  - Gas Chromatography-Mass Spectrometry/*methods
MH  - Insecticides/*analysis
MH  - Pyrethrins/*analysis
MH  - Tandem Mass Spectrometry/methods
EDAT- 2009/03/19 09:00
MHDA- 2009/05/07 09:00
CRDT- 2009/03/19 09:00
PHST- 2009/03/19 09:00 [entrez]
PHST- 2009/03/19 09:00 [pubmed]
PHST- 2009/05/07 09:00 [medline]
AID - 10.1021/jf8032446 [doi]
PST - ppublish
SO  - J Agric Food Chem. 2009 Mar 25;57(6):2096-104. doi: 10.1021/jf8032446.