Molecularly imprinted solid phase extraction of urinary diethyl thiophosphate and diethyl dithiophosphate and their analysis by gas chromatography–mass spectrometry

Santos, Mariane Gonçalves; Vitor, Ricardo Vilela; Andrade, Felipe Lopes; Martins, Ignez Salas; Figueiredo, Eduardo Costa

doi:10.1016/j.jchromb.2012.10.015

Cited by 27 publications

(22 citation statements)

References 32 publications

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“…The artifacts have not been specifically identified. Acceptable results were obtained for the derivatization using microwave as a heating source since the fragmentation patterns are comparable to those obtained by Santos et al [6], Hemakanthi et al [4], De Alwis et al [5], and Schindler et al [8], who using conventional derivatization. The highest peak areas and satisfactory repeatability were observed with the MAD output of 160 W and time 5 min, as showed in Fig.…”

Section: Derivatization Proceduressupporting

confidence: 78%

“…The m/z 181 represented the PFBBr, m/z of 185 and 169 represented DETP and DEDTP. These were also the fragments used by Santos et al [6,12] for identification and quantification.…”

Section: Fragmentation Patterns Of the Dapmentioning

confidence: 99%

“…The ions at m/z 350, 274 and 213 as well as the ions at m/z 366, 185 and 157 were employed to confirm the identity of DETP and DEDTP, respectively. The data files were acquired by GCMS-Solution software R , employing same conditions used by Santos et al [6].…”

Section: Gc-ms Conditionsmentioning

confidence: 99%

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Dialkyl phosphates determination by gas chromatography: Evaluation of a microwave‐assisted derivatization†

Silvério

Machado

Boralli

et al. 2015

J of Separation Science

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Dialkyl phosphates are organophosphate insecticide metabolites and their urinary analysis is useful for assessing human exposure to these compounds. This study presents a sample preparation method with microwave-assisted derivatization for two dialkyl phosphates to make the process faster before gas chromatographic analysis. The optimized conditions for derivatization procedure were: 250 μL of 2,3,4,5,6-pentafluorobenzyl bromide 3% in acetonitrile for derivative; microwave for 5 min with intensity of 160 W. The electron ionization mass spectrometric analysis was performed using a gas chromatography with mass spectrometry QP-2010 from the Shimadzu(®) equipped with RTx(®) -5MS capillary column. Ions were monitored at selected-ion monitoring mode at m/z 350 for diethyl thiophosphate and m/z 366 for diethyl dithiophosphate. The developed method was linear for both metabolites. The intra-assay precision was the values ranged between 1.1 and 9.1%, for diethyl thiophosphate, and between 4.06 and 6.9%, for diethyl dithiophosphate. The interassay precision showed relative standard deviation between 10.3 and 15.1%, for diethyl thiophosphate and between 4.9 and 11.9%, for diethyl dithiophosphate. The results obtained suggests that derivatization assisted by microwave, before gas chromatography with mass spectrometry analysis, can be applied to monitoring of exposure to organophosphates once is fast, sensible, and precise method to determinate dialkyl phosphates.

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Section: Derivatization Proceduressupporting

confidence: 78%

“…The m/z 181 represented the PFBBr, m/z of 185 and 169 represented DETP and DEDTP. These were also the fragments used by Santos et al [6,12] for identification and quantification.…”

Section: Fragmentation Patterns Of the Dapmentioning

confidence: 99%

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Dialkyl phosphates determination by gas chromatography: Evaluation of a microwave‐assisted derivatization†

Silvério

Machado

Boralli

et al. 2015

J of Separation Science

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“…This dummy approach was reported by different groups to produced OPP MIPs [48,49,60,63,80], including the use of a metabolite of OPPs, i.e. DETP [50]. As for other molecules, the most common approach used for the development of OPP MIPs for extraction purposes, consists of a non-covalent imprinting.…”

Section: Synthesis Of Mipsmentioning

confidence: 99%

“…If welldefined cavities were created during the polymerization step, the strength of the interactions is higher on the MIP than on the NIP because the template can be retained by different points (sum of the interactions) due to the spatial complementarities between the template and the cavities. The first evaluation of the synthesized MIPs may consist in characterizing by SEM the surface of MIP/NIP [39,54,77,78,97,102], the shape and size of particles [50,58,59,79,98]. BET adsorption method can also be used to measure and compare the porosity of MIP/NIP [64].…”

Section: Mip Characterizationmentioning

confidence: 99%

Molecularly imprinted polymers for the determination of organophosphorus pesticides in complex samples

Boulanouar

Mezzache

Combès

et al. 2018

Talanta

123

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Organophosphorus compounds constitute an important class of pesticides whose the toxicity of which arises from the inhibition of the acetylcholinesterase enzyme. They exhibit a wide range of physico-chemical properties, thus rendering their determination in complex oil samples particularly difficult. To facilitate their analysis at the trace level in various samples (environmental waters, soils, vegetables…), molecularly imprinted polymers (MIPs) that are synthetic polymers possessing specific cavities designed for a target molecule have been prepared. Often called synthetic antibodies, MIPs can replace antibodies in different application fields. Indeed, as immunosorbents, MIPs can be used as selective sorbents for the solid phase extraction of target analytes from complex matrices or as recognition elements in sensors. Their synthesis, characterization and use as selective sorbent for the selective recognition of organophosphorus pesticides have been already largely described and are summarized in this review.

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Sample Preparation via Molecularly Imprinted Polymers (MIPs) in LC‐MS Bioanalysis

Díaz‐Álvarez¹,

Martín‐Esteban²

2019

Sample Preparation in LC‐MS Bioanalysis

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Molecularly imprinted solid phase extraction of urinary diethyl thiophosphate and diethyl dithiophosphate and their analysis by gas chromatography–mass spectrometry

Cited by 27 publications

References 32 publications

Dialkyl phosphates determination by gas chromatography: Evaluation of a microwave‐assisted derivatization†

Dialkyl phosphates determination by gas chromatography: Evaluation of a microwave‐assisted derivatization†

Molecularly imprinted polymers for the determination of organophosphorus pesticides in complex samples

Sample Preparation via Molecularly Imprinted Polymers (MIPs) in LC‐MS Bioanalysis

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