PMID- 24401454
OWN - NLM
STAT- MEDLINE
DCOM- 20140902
LR  - 20140109
IS  - 1873-3573 (Electronic)
IS  - 0039-9140 (Linking)
VI  - 119
DP  - 2014 Feb
TI  - Application of the experimental design of experiments (DoE) for the determination 
      of organotin compounds in water samples using HS-SPME and GC-MS/MS.
PG  - 544-52
LID - S0039-9140(13)00940-5 [pii]
LID - 10.1016/j.talanta.2013.11.052 [doi]
AB  - When attempting to discover the important factors and then optimise a response by 
      tuning these factors, experimental design (design of experiments, DoE) gives a 
      powerful suite of statistical methodology. DoE identify significant factors and 
      then optimise a response with respect to them in method development. In this 
      work, a headspace-solid-phase micro-extraction (HS-SPME) combined with gas 
      chromatography tandem mass spectrometry (GC-MS/MS) methodology for the 
      simultaneous determination of six important organotin compounds namely 
      monobutyltin (MBT), dibutyltin (DBT), tributyltin (TBT), monophenyltin (MPhT), 
      diphenyltin (DPhT), triphenyltin (TPhT) has been optimized using a statistical 
      design of experiments (DOE). The analytical method is based on the ethylation 
      with NaBEt4 and simultaneous headspace-solid-phase micro-extraction of the 
      derivative compounds followed by GC-MS/MS analysis. The main experimental 
      parameters influencing the extraction efficiency selected for optimization were 
      pre-incubation time, incubation temperature, agitator speed, extraction time, 
      desorption temperature, buffer (pH, concentration and volume), headspace volume, 
      sample salinity, preparation of standards, ultrasonic time and desorption time in 
      the injector. The main factors (excitation voltage, excitation time, ion source 
      temperature, isolation time and electron energy) affecting the GC-IT-MS/MS 
      response were also optimized using the same statistical design of experiments. 
      The proposed method presented good linearity (coefficient of determination 
      R(2)>0.99) and repeatibilty (1-25%) for all the compounds under study. The 
      accuracy of the method measured as the average percentage recovery of the 
      compounds in spiked surface and marine waters was higher than 70% for all 
      compounds studied. Finally, the optimized methodology was applied to real aqueous 
      samples enabled the simultaneous determination of all compounds under study in 
      surface and marine water samples obtained from Valencia region (Spain).
CI  - (c) 2013 Elsevier B.V. All rights reserved.
FAU - Coscolla, Clara
AU  - Coscolla C
AD  - Center for Public Health Research (FISABIO), 21 Avenida Catalunya, 46020 
      Valencia, Spain. Electronic address: coscolla_cla@gva.es.
FAU - Navarro-Olivares, Santiago
AU  - Navarro-Olivares S
AD  - Center for Public Health Research (FISABIO), 21 Avenida Catalunya, 46020 
      Valencia, Spain.
FAU - Marti, Pedro
AU  - Marti P
AD  - Center for Public Health Research (FISABIO), 21 Avenida Catalunya, 46020 
      Valencia, Spain.
FAU - Yusa, Vicent
AU  - Yusa V
AD  - Center for Public Health Research (FISABIO), 21 Avenida Catalunya, 46020 
      Valencia, Spain.
LA  - eng
PT  - Journal Article
DEP - 20131128
PL  - Netherlands
TA  - Talanta
JT  - Talanta
JID - 2984816R
RN  - 0 (Organotin Compounds)
RN  - 0 (Water Pollutants, Chemical)
SB  - IM
MH  - Gas Chromatography-Mass Spectrometry/*methods
MH  - Organotin Compounds/*analysis
MH  - Solid Phase Microextraction/*methods
MH  - Tandem Mass Spectrometry/*methods
MH  - Water Pollutants, Chemical/*analysis
OTO - NOTNLM
OT  - Design of experiments
OT  - GC-MS/MS
OT  - Organotin compounds
OT  - Solid-phase microextraction
OT  - Water analysis
EDAT- 2014/01/10 06:00
MHDA- 2014/09/03 06:00
CRDT- 2014/01/10 06:00
PHST- 2013/07/29 00:00 [received]
PHST- 2013/11/13 00:00 [revised]
PHST- 2013/11/18 00:00 [accepted]
PHST- 2014/01/10 06:00 [entrez]
PHST- 2014/01/10 06:00 [pubmed]
PHST- 2014/09/03 06:00 [medline]
AID - S0039-9140(13)00940-5 [pii]
AID - 10.1016/j.talanta.2013.11.052 [doi]
PST - ppublish
SO  - Talanta. 2014 Feb;119:544-52. doi: 10.1016/j.talanta.2013.11.052. Epub 2013 Nov 
      28.