ABSTRACT
Acetylsalicylic acid (AAS) is a drug utilized as analgesic, anti-inflammatory, and antipyretic medication, available worldwide and commonly used in Brazil. Salicylic acid (AS) is a precursor in AAS synthesis and is also produced during its degradation. The official United States Pharmacopoeia (USP) suggests the determination of these drugs by high performance liquid chromatography (HPLC), with ultraviolet detection, but this method has neither a high sensitivity (S AAS=0.12 mAbs/(μg/mL) and S AS=0.48 mAbs/(μg/mL)) nor resolution (Rs=1.61). The purpose of this study was to develop a new more adequate, accurate method by liquid phase chromatography than the current official methodology, and to use this new method in the determination of the tenors of acetylsalicylic, as of salicylic acids in tablets. The parameters of the chromatographic system for both the AAS and AS were satisfactory. Selectivity was verified by absorption spectra comparison in the ultraviolet (UV) range, during and after substance retention time. The linear range for AAS was 0.21 to 0.39 mg/mL, and that for AS was 6.3 to 11.7 μg/mL. The correlation coefficients (r) of the analytical curves of AAS and AS were 0.9995 and 0.9988, respectively; and the detection and quantification limits for the AS were 0.23 and 0.69 μg/mL. The sensitivity (S AAS=1.88 mAbs/(μg/mL) and S AS=1.84 mAbs/(μg/mL)) and the resolution (Rs =5.06) show the improvement obtained using this method over that described by the USP.
O ácido acetilsalicílico (AAS) é um fármaco utilizado como analgésico, antiinflamatório, antipirético, sendo amplamente comercializado e consumido no Brasil e no mundo. Como precursor de sua síntese utiliza-se o ácido salicílico (AS) que também é produzido através de sua degradação. A metodologia oficial da Farmacopéia Americana (USP) preconiza a determinação destes fármacos por cromatografia líquida de alta eficiência (CLAE) com detecção por ultravioleta, mas este método não possui boa sensibilidade (S AAS=0,12 mAbs/(μg/mL) e S AS=0,48 mAbs/(μg/mL)) e resolução (Rs =1,61). O objetivo deste trabalho, visando a melhor adequação do sistema cromatográfico em relação à metodologia oficial, foi o desenvolvimento e otimização de um novo método por cromatografia em fase líquida para determinar os teores tanto do ácido acetilsalicílico quanto do salicílico em comprimidos. Os parâmetros da adequação do sistema cromatográfico para o AAS e para o AS foram satisfatórios. A seletividade foi verificada por comparações dos espectros de absorção no ultravioleta (UV) antes, durante e depois do tempo de retenção da substância. A faixa linear de trabalho para o AAS foi de 0,21 a 0,39 mg/mL e a do AS foi de 6,3 a 11,7 μg/mL. Os coeficientes de correlação (r) das curvas analíticas do AAS e do AS foram de 0,9995 e 0,9988, respectivamente e os limites de detecção e quantificação para o AS foram 0,23 e 0,69 μg/mL. A sensibilidade (S AAS=1,88 mAbs/(μg/mL) e S AS=1,84 mAbs/(μg/mL)) e a resolução (Rs=5,06) atestam a melhoria em relação ao método descrito na USP.
Subject(s)
Analytic Sample Preparation Methods , Aspirin/analysis , Tablets/analysis , Chromatography, High Pressure Liquid/methods , Technological Development/analysis , Diagnosis/methods , Salicylates , Spectrophotometry, Ultraviolet/methods , PharmacokineticsABSTRACT
PURPOSE: To analyze, in vitro, the effects of acetylsalicylic acid (aspirin) and acetic acid solutions on VX2 carcinoma cells in the liver of rabbits with VX2 hepatic tumors; to determine the histolytic and anatomopathological characteristics of the solutions; and to evaluate the eventual biochemical and hepatic changes. METHODS: A total of 48 rabbits were evaluated. The animals were randomized into two groups, protocol 3 (study group) and protocol 4 (controls), and each group was then subdivided into 3 subgroups. Four days after implantation of the tumor in the liver, median laparotomy was performed with a 0.4-ml injection of a solution of either aspirin (5.0 percent), acetic acid (5.0 percent) or saline. The animals were sacrificed after 24 hours (protocol 3) or after 11 days (protocol 4). Body weight, clinical evolution and biochemical levels, as well as the abdominal and thoracic cavities, were evaluated, and liver microscopy was performed. RESULTS: No changes in clinical evolution, body weight or biochemical levels were reported. However, an increase in alkaline phosphatase was observed in protocol 4 (controls). The tumor was eliminated in both protocols. CONCLUSION: Acetylsalicylic acid and acetic acid solutions cause the destruction of experimental hepatic tumors.
OBJETIVO: Analisar os efeitos das soluções de aspirina e de ácido acético, in vivo, em fígado de coelhos portadores de tumor hepático VX2, verificando o efeito histolítico e anatomo-patológico das soluções e eventuais alterações bioquímicas hepáticas. MÉTODOS: Utilizou-se 48 coelhos, divididos em 2 protocolos experimentais(3 e 4), subdivididos em 3 grupos cada. Após 4 dias da implantação do tumor no fígado, procedeu-se a laparotomia mediana, com injeção de 0,4 ml da solução de aspirina (5,0 por cento), de ácido acético (5,0 por cento) e solução salina; o sacrifício ocorreu apos 24 horas (protocolo 3) e 11 dias (protocolo 4); avaliou-se o peso, evolução clinica, dosagens bioquímicas, cavidade abdominal e torácica e microscopia do fígado. RESULTADOS: Não foram observadas alterações na evolução clinica, peso e nas dosagens bioquímicas, apenas elevação da fosfatase alcalina no grupo controle do protocolo 4. Observamos desaparecimento do tumor em ambos os protocolos. CONCLUSÃO: As soluções de ácido acético e ácido acetilsalicílico acarretam destruição do tumor hepático experimental.
Subject(s)
Animals , Aspirin/administration & dosage , Aspirin/analysis , Aspirin/adverse effects , Rabbits , Laparotomy/methods , Liver Neoplasms/diagnosis , Liver Neoplasms/prevention & controlABSTRACT
De acuerdo con las investigaciones más recientes, los beneficios de la aspirina se extienden a un amplio rango de pacientes que han sobrevivido a un accidente cardiovascular. En cuanto a su uso en personas clínicamente sanas, es todavía cuestión de valoración clínica pero está en progreso un estudio en gran escala que busca aclarar este punto
Subject(s)
Humans , Aspirin/administration & dosage , Aspirin/analysis , Aspirin/classification , Myocardial Infarction/surgery , Myocardial Infarction/diagnosis , Myocardial Infarction/physiopathology , Myocardial Infarction/mortality , Myocardial Infarction/prevention & controlABSTRACT
The objective of this investigation was to prepare more stable controlled release aspirin tablets. This was achieved via incorporation of the drug into solid dispersions using three different carries. The carries selected were stearic acid, sodium stearate and magnesium stearate in different ratios. Solid dispersions were prepared by melting technique. The prepared dispersions were evaluated by various methods viz infrared analysis, X-ray diffraction, thermal analysis and microscopic scanning. The previously prepared solid dispersions were utilized to prepare aspirin tablets. It was found that the release from these tablets was dependent on the drug ratio as well as the matrix type. Aspirin release was found to obey first order kinetics. In addition, the drug release was found to be diffusion controlled at 20%, 40% and 60% drug concentration, while solid dispersions containing 80% drug concentration did not follow Higuchi diffusion model
Subject(s)
Drug Stability , Aspirin/analysis , Drug EvaluationABSTRACT
The simultaneous determination of acetylsalicylic acid (ASA) and its degradation product, salicylic acid (SA) in effervescent tablets by high performance liquid chromatography (HPLC) and UV-multicomponent spectrophotometric (MCS) methods is described. In HPLC method, the analytes were extracted with a mixture of acetic acid and methanol (1:99v/v) and aliquots of these solutions appropriately diluted were injected on a reversed-phase C-18 column using a mobile phase consisting of methanol, water and acetic acid, isocratic elution and detection at 283nm. Recoveries ranging from 98.43 to 101.48 por cento and from 99.13 to 102.80 por cento were obtained from commercial samples for ASA and SA, respectively. Relative standard deviations ranged from 0.94 to 1.31 por cento for ASA and from 1.83 to 2.50 por cento for SA. In MCS method, a mixture of acetic acid and chloroform (1:99v/v) was used as solvent. Analyte solutions were measured at 280 and 310nm. Recoveries ranging from 98.30 to 102.02 por cento and from 98.50 to 103.20 were obtained from commercial samples for ASA and SA, respectively. Relative standard deviations ranged from 0.40 to 0.73 por cento for ASA and from 0.86 to 0.93 por cento for SA. Results were compared statistically by F and t tests. On the basis of precision, accuracy, time saving and economy, MCS method was found to show advantages over the HPLC method and can be applied for routine analysis of commercial samples in quality control laboratories.
Subject(s)
Aspirin/analysis , Chromatography, High Pressure Liquid/methods , Salicylates/analysis , Spectrophotometry , Analgesics , Analgesics, Non-Narcotic , Anti-Inflammatory Agents , Chemistry, Pharmaceutical , Dosage Forms , Quality ControlABSTRACT
Non -aspirin salicylates are potentially toxic when ingested in large quantities. Most of these compounds are metabolized in vivo into salicylates. Therefore, estimation of the amount of the salicylate available in pharmaceutical preparations is needed whenever intoxication is induced by such preparations. The following equations were used to calculate aspirin equivalency of products [Table 1] containing non - aspirin salicylates which are product by the state co. For Drug Industries in Iraq, since such informations are not available
Subject(s)
Aspirin/analysis , Drug EvaluationABSTRACT
Se demuestra mediante su aplicación durante un período de aproximadamente 2 años la factibilidad de establecer sistemáticamente la técnica espectrofotométrica usada para el control de calidad de la aspirina, hallándose su error sistemático (0,02 %) comprendidos los efectos inter e intralaboratorios y se comprobó estadísticamente su concordancia con buena aproximación con respecto al método oficial (USP XXI). La evolución del contenido de ácido salicílico en las muestras objeto de estudio permite recomendar el envase 817 mL y el uso de la materia prima designada "I". De acuerdo con los resultados obtenidos debe esperarse un contenido de salicílico libre inferior a los límites oficiales, al menos, durante año y medio en las condiciones actuales y con las recomendaciones antes mencionadas
Subject(s)
Aspirin/analysis , Quality Control , Salicylates/analysis , SpectrophotometryABSTRACT
Se realiza una revisión bibliográfica de los métodos oficiales en la farmacopeas para la determinación del ácido acetil salicílico y su producto de hidrólisis, el ácido salicílico, así como los descritos por distintos autores. Se hace un estudio de las ventajas e inconvenientes de los mismos. Se desarrolla un método analítico para el control sistemático de las tabletas de producción nacional que permita la determinación cuantitativa del ácido acetil salicílico y del ácido salicílico. Se estudia la estabilidad en distintos solventes para seleccionar el mejor. Se informa que el método es útil para los estudios de estabilidad, pues resulta específico y rápido