PMID- 20694812
OWN - NLM
STAT- MEDLINE
DCOM- 20110103
LR  - 20160512
IS  - 1618-2650 (Electronic)
IS  - 1618-2642 (Linking)
VI  - 398
IP  - 3
DP  - 2010 Oct
TI  - Response surface optimization for determination of pesticide residues in grapes 
      using MSPD and GC-MS: assessment of global uncertainty.
PG  - 1509-23
LID - 10.1007/s00216-010-4046-4 [doi]
AB  - In this work, a simple and low-cost method based on matrix solid-phase dispersion 
      (MSPD) and gas chromatography to determine eight multi-class pesticides such as 
      vinclozolin, dichlofluanid, penconazol, captan, quinoxyfen, fluquinconazol, 
      boscalid, and pyraclostrobin in grapes is described. Fungicide residues were 
      identified and quantified using gas chromatography-mass spectrometry in selected 
      ion monitoring mode (GC-MS, SIM). The experimental variables that affect the MSPD 
      method, such as the amount of solid phase, solvent nature and elution volume were 
      optimized using an experimental design. The best results were obtained using 0.5 
      g of grapes, 1.0 g of silica as clean-up sorbent, 1.50 g of C(18) as bonded phase 
      and 10 mL of dichloromethane/ethyl acetate (1:1, v/v) as eluting solvent. 
      Significant matrix effects observed for most of the pesticides tested were 
      eliminated using matrix-matched standards. The pesticide recoveries in grapes 
      samples were better than 80% except for captan. Intra-laboratory precision in 
      terms of Horwitz ratio of the pesticides evaluated was below 0.5, suggesting 
      ruggedness of the method. The quantification limits of the pesticides were in the 
      range of 3.4-8.7 microg kg(-1), which were lower than the maximum residue limits 
      (MRLs) of the pesticides in grapes samples established by the European 
      legislation. Decision limits (CCalpha) and detection capability (CCbeta) have 
      been calculated. The expanded uncertainties at two levels of concentration were 
      <20% for all analytes.
FAU - Lagunas-Allue, L
AU  - Lagunas-Allue L
AD  - Departamento de Quimica, Universidad de La Rioja, Madre de Dios, 51, 26006, La 
      Rioja, Spain.
FAU - Sanz-Asensio, J
AU  - Sanz-Asensio J
FAU - Martinez-Soria, M T
AU  - Martinez-Soria MT
LA  - eng
PT  - Journal Article
PT  - Research Support, Non-U.S. Gov't
DEP - 20100809
PL  - Germany
TA  - Anal Bioanal Chem
JT  - Analytical and bioanalytical chemistry
JID - 101134327
RN  - 0 (Pesticide Residues)
SB  - IM
MH  - Gas Chromatography-Mass Spectrometry/*methods
MH  - Limit of Detection
MH  - Pesticide Residues/*analysis
MH  - Reproducibility of Results
MH  - Surface Properties
MH  - Uncertainty
MH  - Vitis/*chemistry
EDAT- 2010/08/10 06:00
MHDA- 2011/01/05 06:00
CRDT- 2010/08/10 06:00
PHST- 2010/04/29 00:00 [received]
PHST- 2010/07/19 00:00 [accepted]
PHST- 2010/07/15 00:00 [revised]
PHST- 2010/08/10 06:00 [entrez]
PHST- 2010/08/10 06:00 [pubmed]
PHST- 2011/01/05 06:00 [medline]
AID - 10.1007/s00216-010-4046-4 [doi]
PST - ppublish
SO  - Anal Bioanal Chem. 2010 Oct;398(3):1509-23. doi: 10.1007/s00216-010-4046-4. Epub 
      2010 Aug 9.