HPLC of Fluorescent Products of Acetaminophen Reaction with Peroxidase

McCormick, C P; Shihabi, Zak K.

doi:10.1080/01483919008049240

Cited by 5 publications

(4 citation statements)

References 6 publications

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“…Há citados na literatura diversos métodos para a determinação de paracetamol, dentre estes destacam-se os métodos microbiológico 4 , volumétricos 5 , por quimioluminescência 6 , espectrofotométrico 7 , fluorimétrico 8 , eletroanalíticos [9][10][11][12][13] , espectroeletroquímico 14 , cromatográficos [15][16][17][18][19] e em análise por injeção em fluxo por espectrofotometria no UV 20 e visível [21][22][23] , fluorescência 24 , quimioluminescência 25 , biamperometria 26,27 e espectrofotometria FTIR (do inglês: Fourier transform infrared) 28 .…”

Section: Introductionunclassified

“…O paracetamol não tem atividade anti-inflamatória, mas ainda assim é provavelmente o antipirético-analgésico de segunda escolha, sobretudo para pacientes alérgicos ao ácido acetilsalicílico ou que sofram de úlceras pépticas. Por ser menos tóxico que a fenacetina, o paracetamol acabou substituindo-a em diversas formulações farmacêuticas, sendo habitual administrar doses diárias 1 variando de 0,3 a 1 g.A Farmacopéia Americana (USP-23) 2 recomenda a cromatografia em camada delgada e espectrofotometria para a determinação de paracetamol em preparações farmacêuticas e a A.O.A.C 3 o método espectrofotométrico com detecção em 520 nm.Há citados na literatura diversos métodos para a determinação de paracetamol, dentre estes destacam-se os métodos microbiológico 4 , volumétricos 5 , por quimioluminescência 6 , espectrofotométrico 7 , fluorimétrico 8 , eletroanalíticos 9-13 , espectroeletroquímico 14 , cromatográficos [15][16][17][18][19] e em análise por injeção em fluxo por espectrofotometria no UV 20 e visível [21][22][23] , fluorescência 24 , quimioluminescência 25 , biamperometria 26,27 e espectrofotometria FTIR (do inglês: Fourier transform infrared) 28 .A análise, o conhecimento e a distribuição de analgésico-antipiréticos em produtos farmacêuticos tem-se constituído um dos principais problemas desde que se iniciou a investigação destes compostos. O maior interesse nestas análises está centrado nos produtos naturais, na necessidade destes compostos em seres humanos e seu emprego na indústria farmacêutica.…”

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Determinação espectrofotométrica por injeção em fluxo de paracetamol (acetaminofeno) em formulações farmacêuticas

Aniceto¹,

Fatibello‐Filho²

2002

Quím. Nova

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Recebido em 4/4/01; aceito em 16/8/01 FLOW INJECTION SPECTROPHOTOMETRIC DETERMINATION OF PARACETAMOL (ACETAMINOPHEN) IN PHARMACEUTICAL FORMULATIONS.A flow injection spectrophotometric procedure is proposed for the determination of paracetamol (acetaminophen) in pharmaceutical formulations. Powdered and liquid samples were previously dissolved/diluted in 0.05 mol L -1 hydrochloric acid solution and a volume of 250 µL was injected directly into a carrier stream of this same acid solution, flowing at 2.5 mL min -1 . Paracetamol reacts with sodium hypochlorite forming N-acetyl-p-benzoquinoneimine which then reacts with sodium salicylate in sodium hydroxide solution yielding a blue indophenol dye which was measured at 640 nm in the pH range of 9.5-10.0. Paracetamol was determined in pharmaceutical products in the 1.0 to 100.0 mg L -1 (3.3x10 -6 a 6.6x10 -4 mol L -1 ) concentration range, with a detection limit of 0.5 mg L -1 (1.6x10 -6 mol L -1 ). The recovery of this analyte in five samples ranged from 98.0 to 103.6 %. The analytical frequency was 80 determinations per hour and the RSDs were less than 1% for paracetamol concentrations of 25.0, 50.0 and 75.0 mg L -1 (n=10). A paired t-test showed that all results obtained for paracetamol in commercial formulations using the proposed flow injection procedure and a spectrophotometric batch procedure agree at the 95% confidence level.Keywords: paracetamol; flow injection spectrophotometry; pharmaceutical formulations. INTRODUÇÃOParacetamol é um analgésico-antipirético pertencente à classe dos derivados do p-aminofenol, introduzido no século passado como resultado de pesquisas destinadas a substitutos para acetanilida. Embora possuam propriedades analgésico-antipiréticas, a fenacetina e a acetanilida dão origem à metemoglobina (hemoglobina incapaz de transportar oxigênio), devido à formação de um precursor da anilina. Tanto a acetanilida quanto a fenacetina são metabolizadas a paracetamol, a substância ativa. Outros fármacos dessa classe são a anidoxina, butacetina, etoxazena, fenacetinol, parapropanol e parsalmida 1 .O paracetamol é obtido por acetilação do p-aminofenol com áci-do acético glacial e anidrido acético. Esse fármaco se apresenta como um pó branco, inodoro e ligeiramente hidrossolúvel e as suas atividades analgésicas e antipiréticas são similares às da acetanilida e fenacetina, da qual é metabólito. O paracetamol não tem atividade anti-inflamatória, mas ainda assim é provavelmente o antipirético-analgésico de segunda escolha, sobretudo para pacientes alérgicos ao ácido acetilsalicílico ou que sofram de úlceras pépticas. Por ser menos tóxico que a fenacetina, o paracetamol acabou substituindo-a em diversas formulações farmacêuticas, sendo habitual administrar doses diárias 1 variando de 0,3 a 1 g.A Farmacopéia Americana (USP-23) 2 recomenda a cromatografia em camada delgada e espectrofotometria para a determinação de paracetamol em preparações farmacêuticas e a A.O.A.C 3 o método espectrofotométrico com detecção em 520 nm.Há citados na literatura diversos mét...

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Section: Introductionunclassified

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Determinação espectrofotométrica por injeção em fluxo de paracetamol (acetaminofeno) em formulações farmacêuticas

Aniceto¹,

Fatibello‐Filho²

2002

Quím. Nova

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“…Paracetamol is oxidized to one or more fluorescent compounds by hydrogen peroxide in the presence of horseradish peroxidase [5,6]. If the HPLC mobile phase conditions after PCD are simulated, the fluorescence spectrum in Figure 2 is obtained.…”

Section: Resultsmentioning

confidence: 99%

“…It is known to undergo a variety of oxidation reactions under the action of a wide range of oxidants including iodosobenzene [1], potassium hexacyanoferrate(III) [2,3], complexes of iron(III) with 1,10-phenanthroline [4], and H202 in the presence of horseradish peroxidase [5,6]. It is known to undergo a variety of oxidation reactions under the action of a wide range of oxidants including iodosobenzene [1], potassium hexacyanoferrate(III) [2,3], complexes of iron(III) with 1,10-phenanthroline [4], and H202 in the presence of horseradish peroxidase [5,6].…”

Section: Introductionmentioning

confidence: 99%

Determination of paracetamol (acetaminophen) by HPLC with post-column enzymatic derivatization and fluorescence detection

Meyer

Kärst

2001

Chromatographia

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A novel method is described for the determination of paracetamol (acetaminophen; N-ace@-4-aminophenol) in urine. After reversed-phase HPLC separation, paracetamol is oxidized by H202 with horseradish peroxiclase catalysis. Detection is performed fluorimetrically at an excitation wavelength of 329 nm and an emission wavelength of 435 nm. Urine samples were spiked with paracetamol, diluted, and injected directly without further pretreatment. Under these conditions, the limit of detection was 2 x 10 -s mol L 1, and the limit of quantification was 7 x 10 -s mol L 1. The method was validated by l",,vo different approaches based on HPLC with UV-Vis detection.

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Fluorescence in Organized Assemblies

Hinze¹

2000

Encyclopedia of Analytical Chemistry

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This article provides an overview of the general properties of organized assembly (ordered media) systems such as aqueous surfactant and bile salt micelles, lipid and surfactant vesicles (liposomes) and cyclodextrins (CDs) and summarizes their utilization to enhance the performance of analytical fluorescence measurements. In many instances, organic molecules and metal complex species, when included within a CD cavity or solubilized and bound to surfactant aggregates, exhibit enhanced fluorescence. This gives rise to improved detectability of such analytes. The altered microenvironment within the organized medium is capable of impeding the interfering action of other species (inorganic or organic) present in the sample matrix. This often can improve the selectivity of the analytical method. These benefits of improved sensitivity and selectivity arise from the compartmentalization, isolation and shielding of the excited singlet state of the guest analyte from quenching and nonradiative decay processes as well as prevent side reactions that otherwise can occur in bulk solution (or sample matrix). In addition, organic solvents or time‐consuming extraction steps can be avoided owing to the increased solubility of the nonpolar organic or inorganic reagents and/or analyte molecules in water in the presence of the organized medium; allowing for the use of an aqueous medium to perform the procedure. The possibility of conducting reactions and forming fluorescent organic or metal chelates in micellar (or other organized) media that are not observed in a bulk homogeneous solvent system serves to expand the scope of chemistries that one can consider using to design/develop new, unique and improved fluorescent assays. Numerous representative examples of fluorescent methods for determination of both organic and inorganic analytes are provided which serve to illustrate the advantages and benefits accrued from the use of the micelles, vesicles, liposomes or CDs in such procedures. Some experimental considerations and cautions to keep in mind when utilizing organized media are also delineated. An extensive reference section is provided so that the interested reader can easily refer to such for more detailed information on these systems and topics.

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HPLC of Fluorescent Products of Acetaminophen Reaction with Peroxidase

Cited by 5 publications

References 6 publications

Determinação espectrofotométrica por injeção em fluxo de paracetamol (acetaminofeno) em formulações farmacêuticas

Determinação espectrofotométrica por injeção em fluxo de paracetamol (acetaminofeno) em formulações farmacêuticas

Determination of paracetamol (acetaminophen) by HPLC with post-column enzymatic derivatization and fluorescence detection

Fluorescence in Organized Assemblies

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