PMID- 18155412
OWN - NLM
STAT- MEDLINE
DCOM- 20080501
LR  - 20071224
IS  - 1873-4324 (Electronic)
IS  - 0003-2670 (Linking)
VI  - 607
IP  - 1
DP  - 2008 Jan 21
TI  - Solid-phase microextraction (SPME) for the determination of pyrethroids in 
      cucumber and watermelon using liquid chromatography combined with post-column 
      photochemically induced fluorimetry derivatization and fluorescence detection.
PG  - 74-82
AB  - A sensitive and efficient solid-phase microextraction (SPME) method for the 
      determination of seven pyrethroid insecticides including fenpropathrin, 
      lambda-cyhalothrin, deltamethrin, fenvalerate, permethrin, tau-fluvalinate and 
      bifenthrin in cucumber and watermelon samples using high performance liquid 
      chromatography combined with post-column photochemically induced fluorimetry 
      derivatization and fluorescence detection (SPME-HPLC-PIF-FD) was developed and 
      validated. The optimum SPME conditions were used for the extraction of samples of 
      both matrices (extraction time 30 min, stirring rate 1100 rpm, extraction 
      temperature 65 degrees C, sample pH 3, soaking time 7 min, desorption time 5 min, 
      ACN content 25%, desorption and soaking solvent was the mobile phase and in 
      static mode). The method was validated in terms of limits of detection (LODs) and 
      the limits of quantification (LOQs) in both IUPAC and EURACHEM criteria. LODs and 
      LOQs were achieved in values lower than the maximum residue levels (MRLs) 
      established in the Spanish regulations for all pesticides in this study (MRLs 
      range between 0.01 and 0.1 mg kg(-1) for all pyrethroid insecticides in both 
      matrices). LOQs according to the second criterion were between 1.5 and 5 microg 
      kg(-1) for cucumber; and between 1.3 and 5 microg kg(-1) for watermelon samples. 
      Precision and recovery studies were evaluated at two concentration levels for 
      each matrix. Good precision was obtained and relative standard deviation values 
      were less than 10% in all cases. Recovery values were calculated at 0.05 and 0.5 
      mg kg(-1) levels (n=6) and they ranged between 93% and 108% for cucumber and 
      between 91% and 110% for watermelon samples. Applicability of the method to 
      pyrethroids in cucumber and watermelon of commercial samples was demonstrated.
FAU - Vazquez, P Parrilla
AU  - Vazquez PP
AD  - Department of Analytical Chemistry, University of Almeria, La Canada de San 
      Urbano, 04120 Almeria, Spain. parrilla@ual.es
FAU - Mughari, Ahmed R
AU  - Mughari AR
FAU - Galera, M Martinez
AU  - Galera MM
LA  - eng
PT  - Journal Article
DEP - 20071123
PL  - Netherlands
TA  - Anal Chim Acta
JT  - Analytica chimica acta
JID - 0370534
RN  - 0 (Insecticides)
RN  - 0 (Pyrethrins)
SB  - IM
MH  - Chromatography, Liquid
MH  - Citrullus/*chemistry
MH  - Cucumis sativus/*chemistry
MH  - Fluorescence
MH  - Fluorometry
MH  - Humans
MH  - Insecticides/*analysis/*chemistry
MH  - Pyrethrins/*analysis/*chemistry
MH  - Solid Phase Microextraction/*methods
MH  - Sonication
MH  - Ultraviolet Rays
EDAT- 2007/12/25 09:00
MHDA- 2008/05/02 09:00
CRDT- 2007/12/25 09:00
PHST- 2007/06/21 00:00 [received]
PHST- 2007/09/21 00:00 [revised]
PHST- 2007/11/15 00:00 [accepted]
PHST- 2007/12/25 09:00 [pubmed]
PHST- 2008/05/02 09:00 [medline]
PHST- 2007/12/25 09:00 [entrez]
AID - S0003-2670(07)01909-5 [pii]
AID - 10.1016/j.aca.2007.11.027 [doi]
PST - ppublish
SO  - Anal Chim Acta. 2008 Jan 21;607(1):74-82. doi: 10.1016/j.aca.2007.11.027. Epub 
      2007 Nov 23.