Behaviour of carbamate pesticides in gas chromatography and their determination with solid‐phase extraction and solid‐phase microextraction as preconcentration steps

Carabias‐Martínez, Rita; García-Hermida, César; Rodríguez‐Gonzalo, Encarnación; Ruano‐Miguel, Luis

doi:10.1002/jssc.200400047

Cited by 51 publications

(19 citation statements)

References 33 publications

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“…Isolation and Identification of Metabolites. Since reference compounds were not available, we intended to examine the primary carbaryl metabolites observed in the present investigation by GC/EI-MS. Due to decomposition (McLafferty rearrangement) during injection and on columns, GC analysis of thermolabile parent carbaryl is difficult [21]; carbaryl is usually detected as naphthalen-1-ol. Similar decomposition was expected of primary carbaryl metabolites with intact carbamate moiety.…”

Section: Distributions Of Radioactivitymentioning

confidence: 99%

Comparison of the Biotransformation of the14C-Labelled Insecticide Carbaryl by Non-Transformed and Human CYP1A1-, CYP1A2-, and CYP3A4-Transgenic Cell Cultures ofNicotiana tabacum

Schmidt¹,

Faymonville²,

Gembé³

et al. 2006

C&B

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Transgenic tobacco-cell-suspension cultures expressing separately the human cytochrome P450 monooxygenases CYP1A1, CYP1A2, and CYP3A4 were utilized to study the biotransformation of the 14C-labelled insecticide carbaryl (=naphthalen-1-yl methylcarbamate). The resulting data were compared to similar data from the corresponding non-transformed (NT) tobacco-cell culture and commercially available membrane preparations (Bactosomes) of genetically modified bacteria separately containing the same human P450s. A rapid conversion rate of carbaryl was observed with the CYP1A1 and CYP1A2 cells, where only 49.7 and 0.2% of applied carbaryl (1 mg/l), respectively, remained after 24 h, as compared to 77.7% in the non-transformed culture. Unexpectedly, the corresponding results obtained from the CYP3A4 cultures were not definite. With 25 mg/l of carbaryl and 96 h of incubation, it was proven that the insecticide is also substrate of CYP3A4. This finding was supported by GC/EI-MS analysis of the primary metabolite pattern produced by the isozyme. This consisted of naphthalene-1-ol, N-(hydroxymethyl)carbaryl, 4-hydroxycarbaryl, and 5-hydroxycarbaryl, whereas the main product in non-transformed cells was N-(hydroxymethyl)carbaryl. Data obtained from the CYP1A1, CYP1A2, or CYP3A4 Bactosomes agreed with those of the P450-transgenic tobacco cells. Problems with GC/EI-MS analysis of carbaryl and its metabolites are discussed.

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Section: Distributions Of Radioactivitymentioning

confidence: 99%

Comparison of the Biotransformation of the14C-Labelled Insecticide Carbaryl by Non-Transformed and Human CYP1A1-, CYP1A2-, and CYP3A4-Transgenic Cell Cultures ofNicotiana tabacum

Schmidt¹,

Faymonville²,

Gembé³

et al. 2006

C&B

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“…Basically, pesticide residue analysis is carried out in a sequence of several steps, i. e. (i) extraction by organic sol-vent(s) methods such as liquid-liquid partitioning [4 -8], solid phase micro-extraction [9], matrix solid phase dispersion [10], single drop microextraction [11], supercritical fluid extraction [12,13]; (ii) cleaning-up by column chromatography and/or gel permeation chromatography [14], SPE [5,7,8,15], dispersive SPE [4 -7] or also stirbar sorptive extraction [16]; (iii) concentration according to analytical technique; and (iv) finally the use of sensitive analytical methods. Most of steps are tedious, solvent and time consuming, labor-intensive, rather complex, and generally were not adapted for one particular pesticide class.…”

Section: Introductionmentioning

confidence: 99%

Method for routine screening of pesticides and metabolites in meat based baby‐food using extraction and gas chromatography‐mass spectrometry

Przybylski¹,

Segard

2009

J of Separation Science

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A simple and complete multiresidue method has been developed for the routine determination of 236 pesticides and degradation products, in meat based baby-food. This original approach combines a modified Quick Easy Cheap Effective Rugged and Safe (QuEChERS) sample preparation method using a triple partitioning extraction step with water/ACN/hexane and a system composed of GC with programmable temperature vaporization injector hyphenated to an IT-MS. Detection was performed in full scan mode, with one quantification ion and one identification ion. We firstly report here the hexane addition in the extraction step to eliminate a major part of lipophile co-extracts. Direct consequences were the increasing of method sensitivity and the diminishment of the frequency of maintenance of the analytical instrument. The recovery data were obtained by spiking blank samples at three concentration levels (10, 50 and 200 microg/kg) over five replicates, yielding average recoveries in the range 70-121% with a RSD evaluated between 2-15%. Linearity was fixed in the range of 10-300 microg/kg with determination coefficients (R2) superior or equal to 0.9814 for all target analytes. Best LODs and LOQs were established as 0.03 and 0.1 microg/kg, respectively. Total instrumental analysis of all molecules was carried out in less than 1 h.

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“…Thermal instability and polarity of many carbamates have limited the use of gas chromatography for their determination [25]. This limitation can be eliminated using a previous derivatization step, which involves an increase of the analysis time and less precision in the procedures used.…”

Section: /5mentioning

confidence: 99%

Identification and quantification of carbamate pesticides in dried lime tree flowers by means of excitation-emission molecular fluorescence and parallel factor analysis when quenching effect exists

Rubio

Ortiz

Sarabia

2014

Analytica Chimica Acta

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Please cite this article as: L.Rubio, M.C.Ortiz, L.A.Sarabia, Identification and quantification of carbamate pesticides in dried lime tree flowers by means of excitationemission molecular fluorescence and parallel factor analysis when quenching effect exists, Analytica Chimica Acta http://dx.doi.org/10. 1016/j.aca.2014.02.008 This is a PDF file of an unedited manuscript that has been accepted for publication. As a service to our customers we are providing this early version of the manuscript. The manuscript will undergo copyediting, typesetting, and review of the resulting proof before it is published in its final form. Please note that during the production process errors may be discovered which could affect the content, and all legal disclaimers that apply to the journal pertain. HighlightsHIGHLIGHTS ► Determination of carbamate pesticides in dried lime tree flowers by EEM and PARAFAC ► Quenching effect and overlapping spectra are solved by three way techniques ► The second order property of PARAFAC decomposition is useful to solve problems in EEM ► Using PARAFAC to select the adequate dilution that minimizes the quenching effect ► A procedure to choose a D-optimal design for a multi-analyte standard addition method Abstract A non-separative, fast and inexpensive spectrofluorimetric method based on the second order calibration of excitation-emission fluorescence matrices (EEMs) was proposed for the determination of carbaryl, carbendazim and 1-naphthol in dried lime tree flowers. The trilinearity property of three-way data was used to handle the intrinsic fluorescence of lime flowers and the difference in the fluorescence intensity of each analyte. It also made possible to identify unequivocally each analyte. Trilinearity of the data tensor guarantees the uniqueness of the solution obtained through parallel factor analysis (PARAFAC), so the factors of the decomposition match up with the analytes. In addition, an experimental procedure was proposed to identify, with three-way data, the quenching effect produced by Page 2 of 40 A c c e p t e d M a n u s c r i p t 2/4 the fluorophores of the lime flowers. This procedure also enabled the selection of the adequate dilution of the lime flowers extract to minimize the quenching effect so the three analytes can be quantified. Finally, the analytes were determined using the standard addition method for a calibration whose standards were chosen with a D-optimal design.The three analytes were unequivocally identified by the correlation between the pure spectra and the PARAFAC excitation and emission spectral loadings. The trueness was established by the accuracy line "calculated concentration versus added concentration" in all cases.

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Behaviour of carbamate pesticides in gas chromatography and their determination with solid‐phase extraction and solid‐phase microextraction as preconcentration steps

Cited by 51 publications

References 33 publications

Comparison of the Biotransformation of the14C-Labelled Insecticide Carbaryl by Non-Transformed and Human CYP1A1-, CYP1A2-, and CYP3A4-Transgenic Cell Cultures ofNicotiana tabacum

Comparison of the Biotransformation of the14C-Labelled Insecticide Carbaryl by Non-Transformed and Human CYP1A1-, CYP1A2-, and CYP3A4-Transgenic Cell Cultures ofNicotiana tabacum

Method for routine screening of pesticides and metabolites in meat based baby‐food using extraction and gas chromatography‐mass spectrometry

Identification and quantification of carbamate pesticides in dried lime tree flowers by means of excitation-emission molecular fluorescence and parallel factor analysis when quenching effect exists

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