PMID- 22748376
OWN - NLM
STAT- MEDLINE
DCOM- 20121030
LR  - 20120710
IS  - 1873-3778 (Electronic)
IS  - 0021-9673 (Linking)
VI  - 1249
DP  - 2012 Aug 3
TI  - Strategies for the multi-residue analysis of 100 pesticides by liquid 
      chromatography-triple quadrupole mass spectrometry.
PG  - 164-80
LID - 10.1016/j.chroma.2012.06.028 [doi]
AB  - Analytical strategies for screening, quantitation and confirmation of a group of 
      100 pesticides in fruit and vegetable samples by LC-MS and LC-MS/MS were 
      developed. The pesticides studied belong to different chemical families of 
      herbicides, insecticides and fungicides. A selection of some degradation products 
      was also included. Chromatographic separation was performed using a Zorbax 
      Eclipse XDB-C8 column (150 mm x 4.6 mm and 5 mum particle size), and gradient 
      elution with acetonitrile-water (both with 0.1% formic acid) as mobile phase. 
      LC-MS/MS using highly-selective selected reaction monitoring (H-SRM) acquisition 
      mode monitoring two transitions for each compound showed to be the most sensitive 
      methodology. Quantitation was carried out using matrix-matched standard 
      calibration and good linearity of response was demonstrated (r>0.998). Limits of 
      detection (by acquiring two transitions and with the ion-ratio requirements) 
      ranged between 0.01 and 20 mug/kg were obtained. So, in general, the sensitivity 
      achieved meets the maximum residue levels (MRLs) established by the European 
      Union regulation for food monitoring programs. Pesticide confirmation was carried 
      out following European Union guidelines. In order to prevent false-positives, 
      further confirmatory strategies were proposed. LC-MS in highly-selective selected 
      ion monitoring (H-SIM) mode with accurate mass measurement was used to obtain an 
      orthogonal criterion (exact mass) for confirmation. Accurate mass measurements 
      were always bellow 0.9 mDa for almost all pesticides studied (similar to those 
      described with TOF instruments). A user reversed energy ramp (RER) product ion 
      scan spectra library was generated by means of a data dependent analysis for 
      routine library searching of pesticides. The combination of LC-MS/MS in H-SRM 
      mode and the generation of the RER product ion scan spectra and library search 
      were then used to achieve further confirmation on pesticide analysis. The LC-MS 
      and LC-MS/MS strategies developed were successfully applied for the analysis and 
      confirmation of pesticides in different types of fruit and vegetables samples, 
      and examples of the screening, quantitation and confirmation of pesticides in 
      these samples are shown in this work.
CI  - Copyright (c) 2012 Elsevier B.V. All rights reserved.
FAU - Nunez, Oscar
AU  - Nunez O
AD  - Department of Analytical Chemistry, University of Barcelona, Marti i Franques, 
      1-11, E-08028, Barcelona, Spain. oscar.nunez@ub.edu
FAU - Gallart-Ayala, Hector
AU  - Gallart-Ayala H
FAU - Ferrer, Imma
AU  - Ferrer I
FAU - Moyano, Encarnacion
AU  - Moyano E
FAU - Galceran, Maria Teresa
AU  - Galceran MT
LA  - eng
PT  - Journal Article
PT  - Research Support, Non-U.S. Gov't
DEP - 20120616
PL  - Netherlands
TA  - J Chromatogr A
JT  - Journal of chromatography. A
JID - 9318488
RN  - 0 (Pesticide Residues)
SB  - IM
MH  - Calibration
MH  - Chromatography, Liquid/*methods
MH  - Fruit/chemistry
MH  - Limit of Detection
MH  - Mass Spectrometry/*methods
MH  - Pesticide Residues/*analysis
MH  - Vegetables/chemistry
EDAT- 2012/07/04 06:00
MHDA- 2012/10/31 06:00
CRDT- 2012/07/04 06:00
PHST- 2012/05/08 00:00 [received]
PHST- 2012/06/07 00:00 [revised]
PHST- 2012/06/10 00:00 [accepted]
PHST- 2012/07/04 06:00 [entrez]
PHST- 2012/07/04 06:00 [pubmed]
PHST- 2012/10/31 06:00 [medline]
AID - S0021-9673(12)00904-1 [pii]
AID - 10.1016/j.chroma.2012.06.028 [doi]
PST - ppublish
SO  - J Chromatogr A. 2012 Aug 3;1249:164-80. doi: 10.1016/j.chroma.2012.06.028. Epub 
      2012 Jun 16.