PMID- 18346746
OWN - NLM
STAT- MEDLINE
DCOM- 20080708
LR  - 20171116
IS  - 0021-9673 (Print)
IS  - 0021-9673 (Linking)
VI  - 1188
IP  - 2
DP  - 2008 Apr 25
TI  - Simultaneous determination of traces of pyrethroids, organochlorines and other 
      main plant protection agents in agricultural soils by headspace solid-phase 
      microextraction-gas chromatography.
PG  - 154-63
LID - 10.1016/j.chroma.2008.02.080 [doi]
AB  - A solvent-free and simple method based on headspace solid-phase microextraction 
      (HS-SPME) was developed in order to determine simultaneously 36 common pesticides 
      and breakdown products (mostly pyrethroids and organochlorine compounds) in soil. 
      The analysis was carried out by gas chromatography with micro-electron-capture 
      detection (GC-microECD). As far as we know, this is the first study about the 
      SPME of pyrethroid insecticides from soil. Factors such as extraction 
      temperature, matrix modification by addition of water, salt addition (% NaCl) and 
      fiber coating were considered in the optimization of the HS-SPME. To this end, a 
      3 x 2(3-1) fractional factorial design was performed. The results showed that 
      temperature and fiber coating were the most significant variables affecting 
      extraction efficiency. A suitable sensitivity for all investigated compounds was 
      achieved at 100 degrees C by extracting soil samples wetted with 0.5 mL of 
      ultrapure water (0% NaCl) employing a polyacrylate (PA) coating fiber. Using the 
      recommended extraction conditions with GC-microECD, a linear calibration could be 
      achieved over a range of two orders of magnitude for both groups of analytes. 
      Limits of detection (LODS) at the sub-ng g(-1) level were attained and relative 
      standard deviations (RSDs) were found to be lower than 14% for both groups of 
      pesticides. Matrix effects were investigated by the analysis of different soil 
      samples fortified with the target compounds. The method accuracy was assessed and 
      good recovery values (>70%, in most cases) were obtained. The method was also 
      validated with a certified reference material (RTC-CRM818-050), which was 
      quantified using a standard addition protocol. Finally, the proposed 
      HS-SPME-GC-microECD methodology was further applied to the screening of 
      environmental soil samples for the presence of the target pesticides.
FAU - Fernandez-Alvarez, Maria
AU  - Fernandez-Alvarez M
AD  - Departamento de Quimica Analitica, Nutricion y Bromatologia, Instituto de 
      Investigacion y Analisis Alimentario, Campus Sur, Universidad de Santiago de 
      Compostela, E-15706 Santiago de Compostela, Spain.
FAU - Llompart, Maria
AU  - Llompart M
FAU - Lamas, J Pablo
AU  - Lamas JP
FAU - Lores, Marta
AU  - Lores M
FAU - Garcia-Jares, Carmen
AU  - Garcia-Jares C
FAU - Cela, Rafael
AU  - Cela R
FAU - Dagnac, Thierry
AU  - Dagnac T
LA  - eng
PT  - Journal Article
PT  - Research Support, Non-U.S. Gov't
DEP - 20080302
PL  - Netherlands
TA  - J Chromatogr A
JT  - Journal of chromatography. A
JID - 9318488
RN  - 0 (Hydrocarbons, Chlorinated)
RN  - 0 (Pesticides)
RN  - 0 (Pyrethrins)
RN  - 0 (Soil)
RN  - 0 (Solvents)
SB  - IM
MH  - *Agriculture
MH  - Chromatography, Gas
MH  - Hydrocarbons, Chlorinated/*analysis
MH  - Pesticides/*analysis/isolation & purification
MH  - Pyrethrins/*analysis
MH  - Reference Standards
MH  - Reproducibility of Results
MH  - Soil/*analysis
MH  - Solid Phase Microextraction/*methods
MH  - Solvents
MH  - Temperature
EDAT- 2008/03/19 09:00
MHDA- 2008/07/09 09:00
CRDT- 2008/03/19 09:00
PHST- 2007/12/14 00:00 [received]
PHST- 2008/02/22 00:00 [revised]
PHST- 2008/02/22 00:00 [accepted]
PHST- 2008/03/19 09:00 [pubmed]
PHST- 2008/07/09 09:00 [medline]
PHST- 2008/03/19 09:00 [entrez]
AID - S0021-9673(08)00395-6 [pii]
AID - 10.1016/j.chroma.2008.02.080 [doi]
PST - ppublish
SO  - J Chromatogr A. 2008 Apr 25;1188(2):154-63. doi: 10.1016/j.chroma.2008.02.080. 
      Epub 2008 Mar 2.