A liquid chromatography–tandem mass spectrometry confirmatory assay for the simultaneous determination of several tetracyclines in milk considering keto–enol tautomerism and epimerization phenomena

Spisso, Bernardete Ferraz; Júnior, Marcus Antônio Gonçalves de Araújo; Monteiro, Mychelle Alves; Lima, Adélia Mara Belém; Pereira, Mararlene Ulberg; Luiz, Robson Alves; Nóbrega, Armi Wanderley da

doi:10.1016/j.aca.2009.10.012

Cited by 41 publications

(13 citation statements)

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“…USEPA Method 1694 guidelines establishes that any chromatographic gradient may be applied for the separation of the pharmaceutical compounds as long as the last eluting peak has a retention time greater than that obtained in the standard USEPA method [19] [24]. Gradient elution for chromatographic separation of tetracyclines was the same described by Spisso et al [3]. For sulfonamide separation, another gradient was developed based on that employed for tetracyclines, due to the physicochemical similarities.…”

Section: Lc Methods Developmentmentioning

confidence: 99%

“…Multiple Reaction Monitoring (MRM) experiments for tetracycline analysis in electrospray positive-ion mode (ESI+) were described by Spisso et al [3] and the employed conditions are listed in Table 3.…”

Section: Lc/ms-ms Instrumentationmentioning

confidence: 99%

“…Antimicrobials were eluted with two portions of 2 mL methanol and two portions of 2 mL ACE:MeOH (1:1, v/v), using gravity flow only. 1 mL aliquots of the eluate were transferred to two centrifuge tubes and evaporated to dryness under N 2 in a temperature up to 47.5˚C, using an evaporator with nitrogen flow (Pierce Reacti-Therm III TM transferred to amber auto-sampler vials for the injection of 10 µL (TC) and 20 µL (SF) [3] [7]. In order to calculate method recoveries, 25 mL of a solution at 100 ng•L −1 (TC and SF) and 25 mL of ultrapure water were used.…”

Section: Sample Collection and Preparationmentioning

confidence: 99%

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Occurrence of Antimicrobials in River Water Samples from Rural Region of the State of Rio de Janeiro, Brazil

Monteiro¹,

Spisso²,

Santos³

et al. 2016

JEP

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The occurrence of antimicrobials in the aquatic environment and drinking water has raised the question of their impact on the environment and public health. Animal production is one of the most expressive activities of Brazilian agribusiness. In order to ensure the productivity and competitiveness of the sector, the use of drugs for therapeutic and prophylactic purposes is a common practice. Due to the continuous release of antimicrobials into the environment, the aim of this study was to compare the frequency of detection of tetracyclines and sulfonamides in surface water collected from rural areas in Lidice District of Rio Claro, in the State of Rio de Janeiro, Brazil. An investigative study was conducted with 24 river water samples analyzed by high-performance liquid chromatography coupled to tandem mass spectrometry and the aim of this study was to determine residues of sulfonamides and tetracyclines based on the USEPA me- M. A. Monteiro et al.231

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Section: Lc Methods Developmentmentioning

confidence: 99%

Section: Lc/ms-ms Instrumentationmentioning

confidence: 99%

Section: Sample Collection and Preparationmentioning

confidence: 99%

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Occurrence of Antimicrobials in River Water Samples from Rural Region of the State of Rio de Janeiro, Brazil

Monteiro¹,

Spisso²,

Santos³

et al. 2016

JEP

Self Cite

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“…[12][13][14][15] Conhecer a concentração de um tautômero não necessariamente satisfaz às necessidades dos ensaios de controle de qualidade, visto que na legislação não há informação sobre as concentrações limites para cada tautômero, nem sobre as proporções entre eles.…”

Section: Introductionunclassified

Influência de processos antagônicos no desenvolvimento de sistema de análises em fluxo para a determinação espectrofotométrica de propiltiouracil em medicamentos

2013

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. A multi-commuted flow system was developed to determine propylthiouracil (PTU) based on the reaction of its thiol form with iminoquinone radical generated by the oxidation of N,N-dimethyl-p-phenylenediamine in an alkaline medium. PTU can be found in tautomeric forms and the tautomeric equilibrium was displaced to enhance the thiol form. However, the reaction product is unstable and its residence time in the flow path was carefully investigated. The proposed procedure showed good precision (< 1.5%) and a limit of detection (3s) of 0.11 mg L -1 . High recoveries were obtained in the validation test. The procedure was employed for propylthiouracil determination in medications.Keywords: tautomeric equilibrium; antagonist processes; propylthiouracil. INTRODUÇÃOAs novas tecnologias, os investimentos nas pesquisas, a ampliação da produção e a facilitação das condições para a aquisição de medicamentos pela população foram algumas das causas que explicam a expansão da indústria farmacêutica. Esse crescimento acarreta também a necessidade de se estabelecer protocolos para a quantificação dos fármacos presentes nos medicamentos que estão disponíveis no mercado.1 Por vezes, as farmacopeias fornecem apenas os protocolos para a determinação da pureza do princípio ativo na matéria-prima, sem trazer detalhes referentes a procedimentos que permitam a avaliação dos mesmos fármacos nas formas em que os medicamentos são comercializados. Essa dificuldade pode ser exemplificada pelo propiltiouracil (PTU), para o qual há poucos métodos analíticos disponíveis.2-7 O PTU é o princípio ativo de medicamentos usados no tratamento do hipertireoidismo. Ele tem sido usado desde a década de 1950 e seu mecanismo de ação se baseia na inibição da síntese da tiroxina (T4) e da tri-iodotironina (T3), pela remoção do iodo livre numa das etapas da bioprodução desses hormônios. 8 Mais recentemente, o PTU foi adotado como referência de amargor e aplicado em estudos sobre a transmissão genética da sensibilidade gustativa e em investigações sobre hábitos alimentares. 9A carência de métodos para a determinação de PTU se justifica pelo fato desse composto existir em equilíbrio tautomérico. Diferentemente de outras isomerias, a tautomeria se caracteriza por equilíbrios dinâ-micos regidos pela interconversão de espécies através de rearranjos intramoleculares de átomos de hidrogênio (como no caso do PTU) ou de heteroátomos.10 As proporções entre os tautômeros numa solução são fortemente afetadas por fatores estruturais, pelo sistema solvente e pelo pH do meio. Assim, a reatividade de um tautômero será drasticamente afetada com pequenas alterações nas condições do meio reacional.11 No caso do propiltiouracil, observa-se no equilíbrio tautomérico (Figura 1) a alteração da função tioamida para um grupo tiol (I a III), aumentando a reatividade da molécula e possibilitando que reações características para compostos tiólicos venham a ocorrer.Caso o objetivo analítico seja quantificar uma das espécies em equilíbrio tautomérico, os procedimentos analíticos serão com...

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“…22 Due to its high sensitivity and selectivity, HPLC coupled to mass spectrometry (MS) or tandem mass spectrometry (MS/MS) 23,24 is becoming more commonly used in the analysis of TCs in very complex samples such as milk, waste water and animal tissues. MS detection with high sensitivity and accurate quantication is the method selected in this study.…”

Section: Introductionmentioning

confidence: 99%

Magnetic solid phase extraction based on graphene oxide/nanoscale zero-valent iron for the determination of tetracyclines in water and milk by using HPLC-MS/MS

Wei

Zhu

2017

RSC Adv.

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A magnetic solid-phase extraction (MSPE) based on graphene oxide/nanoscale zero-valent iron (GO/nZVI) coupled with high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) was proposed for the determination of trace tetracycline antibiotics (TCs) in water and milk. GO covered nZVI was self-assembled by electrostatic forces by varying the pH. Several important parameters affecting the MSPE procedure have been investigated. The pH value is a key factor in the whole MSPEprocess. An appropriate pH can not only improve adsorption and desorption efficiency, but also enable the extraction of TCs from GO/nZVI by using deionized water. Optimal conditions were then used for the extraction of TCs from real samples, prior to HPLC-MS/MS determination in the positive ESI mode of multiple reaction monitoring (MRM) using a ZORBAX Eclipse Plus C 18 column. The proposed method achieved low limits of quantitation in the range of 8.05-83.19 ng L À1 and 17.42-182.75 ng L À1 for water and milk samples, respectively, and satisfactory recoveries in the range of 84.2-105.5% with intra-day RSD in the range of 0.6-2.5% and inter-day RSD in the range of 1.2-9.2% for the spiked water sample and from 87.0% to 101.8% with intra-day RSD in the range of 1.1-5.4% and inter-day RSD in the range of 2.0-9.7% for the spiked milk sample.

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A liquid chromatography–tandem mass spectrometry confirmatory assay for the simultaneous determination of several tetracyclines in milk considering keto–enol tautomerism and epimerization phenomena

Cited by 41 publications

References 44 publications

Occurrence of Antimicrobials in River Water Samples from Rural Region of the State of Rio de Janeiro, Brazil

Occurrence of Antimicrobials in River Water Samples from Rural Region of the State of Rio de Janeiro, Brazil

Influência de processos antagônicos no desenvolvimento de sistema de análises em fluxo para a determinação espectrofotométrica de propiltiouracil em medicamentos

Magnetic solid phase extraction based on graphene oxide/nanoscale zero-valent iron for the determination of tetracyclines in water and milk by using HPLC-MS/MS

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