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1.
Luminescence ; 33(6): 1026-1032, 2018 Sep.
Artigo em Inglês | MEDLINE | ID: mdl-29927539

RESUMO

One of the most commonly used drugs in treatment of schizophrenia is flupentixol dihydrochloride, therefore it is important to develop a simple, low cost and sensitive spectrofluorimetric method for the estimation of flupentixol dihydrochloride. The yellow fluorescent product that is generated from the nucleophilic substitution reaction of the free lone pair of the alcoholic hydroxyl group of the drug and 4-chloro-7-nitrobenzofurazan (NBD-Cl) in Mcllvaine buffer pH 7.0 was estimated at 510 nm (λex 460 nm). The variables that affect the development of the reaction product were explored and optimized. The linear range of this method was 0.5-2.5 µg ml-1 with a limit of quantitation equal to 0.29 µg ml-1 . Our method was successfully applied for the assurance of flupentixol in tablet form with average percentage recovery of 99.08 ± 1.01% without obstruction from the basic excipients exhibits. Furthermore, our strategy was extended to study the content uniformity testing of flupentixol in Fluaxnol® tablets.


Assuntos
Benzoxazóis/química , Corantes Fluorescentes/química , Flupentixol/análise , Ácido Clorídrico/análise , Estrutura Molecular , Espectrometria de Fluorescência
2.
Anal Bioanal Chem ; 408(4): 1249-58, 2016 Feb.
Artigo em Inglês | MEDLINE | ID: mdl-26677021

RESUMO

The postmortem redistribution (PMR) phenomenon complicates interpretation in forensic toxicology. Human data on time-dependent PMR are rare and only exist for blood so far. A new method for investigation of time-dependent PMR in blood as well as in alternative body fluids and tissues was developed and evaluated using automated biopsy sampling. At admission of the bodies, introducer needles were placed in liver, lung, kidney, muscle, spleen, adipose tissue, heart, femoral vein, and lumbar spine using a robotic arm guided by a computed tomography scanner (CT). Needle placement accuracy was analyzed and found to be acceptable for the study purpose. Tissue biopsies and small volume body fluid samples were collected in triplicate through the introducer needles. At autopsy (around 24 h after admission), samples from the same body regions were collected. After mastering of the technical challenges, two authentic cases were analyzed as a proof of concept. Drug concentrations of venlafaxine, O-desmethylvenlafaxine, bromazepam, flupentixol, paroxetine, and lorazepam were determined by LC-MS/MS, and the percentage concentration changes between the two time points were calculated. Concentration changes were observed with both increases and decreases depending on analyte and matrix. While venlafaxine, flupentixol, paroxetine, and lorazepam generally showed changes above 30% and more, O-desmethylvenlafaxine and bromazepam did not undergo extensive PMR. The presented study shows that CT-controlled biopsy collection provides a valuable tool for systematic time-dependent PMR investigation, demanding only minimal sample amount and causing minimal damage to the body.


Assuntos
Biópsia Guiada por Imagem/métodos , Mudanças Depois da Morte , Autopsia , Cromatografia Líquida , Succinato de Desvenlafaxina/análise , Desenho de Equipamento , Feminino , Flupentixol/análise , Toxicologia Forense/métodos , Humanos , Biópsia Guiada por Imagem/instrumentação , Lorazepam/análise , Pessoa de Meia-Idade , Paroxetina/análise , Robótica/instrumentação , Espectrometria de Massas em Tandem , Fatores de Tempo , Distribuição Tecidual , Tomografia Computadorizada por Raios X , Cloridrato de Venlafaxina/análise
3.
Luminescence ; 31(5): 1091-7, 2016 Aug.
Artigo em Inglês | MEDLINE | ID: mdl-26669624

RESUMO

A reliable, sensitive, cheap and non-extractive spectrofluorimetric method has been developed and validated for determination of thioridazine and flupentixol based on ternary complex formation with eosin and lead(II) in the presence of methylcellulose as surfactant at pH 3.2. Under the optimum conditions, the quantitative quenching effect of investigated drugs on the native fluorescence of eosin has been investigated. The quenching of the eosin fluorescence was measured at 517 nm after excitation at 462 nm. The different experimental parameters affecting the development and stability of the reaction products were carefully studied and optimized, and the results were satisfactory. The calibration plots were constructed over the range of 0.5-3.0 µg mL(-1) . The developed method was successfully applied for determination of investigated drugs in commercial tablets without interference from common excipients. It was further applied for content uniformity testing of flupentixol in its tablets. Statistical comparisons of the results with those of the reference methods revealed excellent agreement and indicated no significant difference in accuracy and precision. Copyright © 2015 John Wiley & Sons, Ltd.


Assuntos
Flupentixol/análise , Tioridazina/análise , Estrutura Molecular , Espectrometria de Fluorescência , Comprimidos/química
4.
Appl Spectrosc ; 69(3): 323-31, 2015 Mar.
Artigo em Inglês | MEDLINE | ID: mdl-25760291

RESUMO

Many pharmaceuticals include highly potent active pharmaceutical ingredients (API), which only require a small dosage to obtain the desired therapeutic effect. This leads to a challenge for quantification of the API using process analytical technology, since the standard nondestructive measurement technique, near-infrared spectroscopy, is not able to quantify below 1% (weight/weight (w/w)) API content. In formulations with more than one API, this challenge is further increased. The purpose of this study is to scrutinize the potential of fluorescence spectroscopy for the simultaneous quantification of two APIs: flupentixol (FLU) in low dosage (0.208-0.625% w/w free base) and melitracen (MEL) (4.17-12.5% w/w free base) in a tablet formulation. Despite internal quenching between the ingredients and the two APIs, this paper demonstrates that it is possible to establish calibrations using partial least squares (PLS) regression on unfolded fluorescence landscapes with a root mean square error of prediction and relative error of 0.038% (w/w) and 9.1%, for FLU and 0.344% (w/w) and 4.1% for MEL, respectively.


Assuntos
Antracenos/análise , Flupentixol/análise , Espectrometria de Fluorescência/métodos , Espectroscopia de Luz Próxima ao Infravermelho/métodos , Comprimidos/química , Tecnologia Farmacêutica/métodos , Algoritmos , Antracenos/química , Flupentixol/química , Reprodutibilidade dos Testes , Sensibilidade e Especificidade , Comprimidos/análise
5.
J Pharm Biomed Anal ; 52(1): 51-8, 2010 May 01.
Artigo em Inglês | MEDLINE | ID: mdl-20060676

RESUMO

Compared to conventional means of quantitative drug analysis, NMR spectroscopy only provides a limited set of adjustable parameters to enhance the quality of the analysis such as pH value, temperature, auxiliary reagents, magnetic field strength or properties of the solvent. In this work we investigate the influence of the kind of solvent on the signal separation of decisive resonances in the NMR spectra of codergocrine mesilate and flupentixol dihydrochloride. Polarity and aromaticity of the solvent play a crucial role in the optimization of signal separation. However, the set of applicable solvents is usually limited due to certain boundary conditions like solubility of the agent. Therefore the effects of solubilizers as well as mixtures solvents on the chemical shift also have to be taken into account. The quantitative results obtained by means of (1)H NMR spectroscopy were found to be in good agreement with the results carried out using official HPLC methods of International Pharmacopoeias.


Assuntos
Cromatografia Líquida de Alta Pressão , Ergotaminas/análise , Flupentixol/análise , Espectroscopia de Ressonância Magnética , Solventes/química , Tecnologia Farmacêutica/métodos , Cromatografia Líquida de Alta Pressão/normas , Excipientes/química , Guias como Assunto , Espectroscopia de Ressonância Magnética/normas , Solubilidade , Tecnologia Farmacêutica/normas
6.
Anal Sci ; 17(11): 1257-61, 2001 Nov.
Artigo em Inglês | MEDLINE | ID: mdl-11759505

RESUMO

A flow-injection (FI) methodology using tris(2,2'-dipyridyl)ruthenium(II), [Ru(dipy)3(2+)], chemiluminescence (CL) was developed for the rapid and sensitive determination of three thioxanthene derivatives, namely zuclopenthixol hydrochloride, flupentixol hydrochloride and thiothixene. The method is based on the CL reaction of the studied thioxanthenes with [Ru(dipy)3(2+)] and Ce(IV) in a sulfuric acid medium. Under the optimum conditions, calibration graphs were obtained over the concentration ranges 0.002-6 migrograms/ml for zuclopenthixol hydrochloride, 0.5-15 micrograms/ml for flupentixol hydrochloride and 0.05-7.5 micrograms/ml for thiothixene. The limits of detection (s/n = 3) were 4.2 x 10(-9) mol/l zuclopenthixol hydrochloride, 2 x 10(-8) mol/l flupentixol hydrochloride and 4.5 x 10(-8) mol/l thiothixene. The method was successfully applied to the determination of these compounds in dosage forms and biological fluids.


Assuntos
Antipsicóticos/análise , Clopentixol/análise , Flupentixol/análise , Tiotixeno/análise , Antipsicóticos/sangue , Antipsicóticos/urina , Césio , Clopentixol/sangue , Clopentixol/urina , Análise de Injeção de Fluxo , Flupentixol/sangue , Flupentixol/urina , Medições Luminescentes , Compostos Organometálicos , Oxirredução , Compostos de Rutênio , Tiotixeno/sangue , Tiotixeno/urina
7.
Eur J Clin Pharmacol ; 35(2): 217-20, 1988.
Artigo em Inglês | MEDLINE | ID: mdl-3191943

RESUMO

Flupenthixol (FP), nortriptyline (NT) and zuclopenthixol, (ZCP) were determined in breast milk and plasma from 2 puerperal, lactating women with psychiatric disorders. The milk concentrations were equal to, higher and lower than those in plasma for FP, NT and ZCP, respectively. Variation in milk triglyceride concentration, but not milk pH, could partly explain between-breast differences in the milk concentrations. The study demonstrates the need for appropriate and representative milk sampling procedures. The estimated daily infant exposure averaged 0.5, 2.3 and 0.3% of the corresponding maternal weight related doses of FP, NT and ZCP. FP was also detectable in infant plasma. These drugs are not known to be harmful in small doses to breast-fed infants. However, concern about the effect of dopamine blocking agents on neurobehavioral mechanisms in animals warrants caution. If neuroleptics are required for a long period this risk must be weighed against the benefits of breast-feeding, also considering the psychological effects of the latter.


Assuntos
Clopentixol/análise , Flupentixol/análise , Leite Humano/análise , Nortriptilina/análise , Tioxantenos/análise , Adulto , Mama/fisiologia , Clopentixol/sangue , Clopentixol/uso terapêutico , Feminino , Flupentixol/sangue , Flupentixol/uso terapêutico , Humanos , Concentração de Íons de Hidrogênio , Lactação , Nortriptilina/sangue , Nortriptilina/uso terapêutico , Gravidez , Transtornos Psicóticos/tratamento farmacológico , Transtornos Puerperais/tratamento farmacológico , Fatores de Tempo , Triglicerídeos/análise
8.
Aust N Z J Psychiatry ; 21(3): 327-38, 1987 Sep.
Artigo em Inglês | MEDLINE | ID: mdl-3435373

RESUMO

Twenty-six chronic schizophrenic patients on well-established depot neuroleptic regimes with stable doses (16 on fluphenazine decanoate, 10 on flupenthixol decanoate) had serum neuroleptic levels measured by radioreceptor assay (RRA) and were followed for six months. The serum prolactin (PRL) concentration and resting electrocardiogram (ECG) were also taken at the beginning of the study period. Correlations had previously been noted between RRA measured neuroleptic levels and outcome in both acute and chronic patients on oral medication. However, in this study of depot medication no significant correlations were found between serum neuroleptic concentration, serum prolactin concentration and the clinical state or outcome. The prevalence (33%) and type of ECG abnormality observed was similar to that previously reported.


Assuntos
Flupentixol/uso terapêutico , Flufenazina/análogos & derivados , Prolactina/sangue , Esquizofrenia/tratamento farmacológico , Tioxantenos/uso terapêutico , Adulto , Preparações de Ação Retardada , Relação Dose-Resposta a Droga , Eletrocardiografia , Feminino , Flupentixol/análogos & derivados , Flupentixol/análise , Flupentixol/farmacocinética , Flufenazina/análise , Flufenazina/farmacocinética , Flufenazina/uso terapêutico , Coração/fisiopatologia , Humanos , Masculino , Pessoa de Meia-Idade , Ensaio Radioligante , Esquizofrenia/sangue , Esquizofrenia/fisiopatologia
9.
Psychopharmacology (Berl) ; 72(1): 107-8, 1980.
Artigo em Inglês | MEDLINE | ID: mdl-6781000

RESUMO

A venous blood sample and an umbilical cord blood sample were obtained from five young women treated with the neuroleptic drug, cis(Z)-flupentixol decanoate in Viscoleo (intramuscularly) or flupentixol (orally) at the time of giving birth. In two cases amniotic fluid was also obtained, and from three of the mothers milk and simultaneous blood samples were obtained in the lactation period. Concentrations of the active drug, cis(Z)-flupentixol were measured in serum, amniotic fluid, and milk by radioimmunoassay. It was found that the concentration of the active drug in umbilical cord serum (fetal serum) was lower than that in serum from the mother--the ratio being about 0.24. Thus the amounts of drug reaching the fetus are low, but they cannot be considered unimportant. The concentrations found in milk were about 30% higher than the serum concentrations. However, the amounts of drug administered to the neonate with the milk are very low and, unless the neonate differs considerably from the adult as to sensitivity to or metabolism of this particular drug, they are of no importance.


Assuntos
Sangue Fetal/análise , Flupentixol/análise , Leite Humano/análise , Tioxantenos/análise , Adulto , Líquido Amniótico/análise , Feminino , Flupentixol/sangue , Humanos , Gravidez
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