Development And Validation Of Hplc Method For Simultaneous Estimation Of Sertaconazole Nitrate And Zinc Pyrithione In Combined Dosage Form

Drugs like Sertraconazole nitrate and Zinc Pyrithion were analyzed by manymethods individually viz HPLC (High performance liquid chromatography) etc but there is nosingle method reported for the simultaneous determination of Sertraconazole nitrate and ZincPyrithion in combination. Although Sertraconazole nitrate is official in British Pharmacopoeiabut Zinc Pyrithion is not official in any Pharmacopoeia. Hence a proper research work is wellaimed to develop and validate a new analytical method for simultaneous estimation ofSertraconazole nitrate and zinc Pyrithion in Pharmaceutical Dosage form.

Development of a microcomposite with single-walled carbon nanotubes and Nd2O3 for determination of paracetamol in pharmaceutical dosage by adsorptive voltammetry / 药物分析学报

This study presents for the first time a new composite of carbon paste (CP), single-walled carbon na-notubes (SWCNTs) and Nd2O3 (NdOX). This versatile composite (NdOX-SWCNT/CPE) was applied to the oxidation of paracetamol (PCM). The newly formed surface was characterized by scanning electron microscopy (SEM), electrochemical impedance spectroscopy (EIS) and cyclic voltammetry (CV). The re-sults showed greater conductivity and a higher surface area for the composite than those of the carbon paste alone. Moreover, the anodic peak currents for PCM increased from 1.6 to 3.6 mA with CPE and NdOX-SWCNT/CPE, indicating an increase of nearly 51.0％ for the anodic peak current. On the other hand, the anodic peak potentials shifted from 0.67 to 0.57 V. The detection limits were 0.05 mmol/L with NdOX-SWCNT/CPE and 0.50 mmol/L with SWCNT/CPE. The relative standard deviations (RSDs) were 1.5％(n =7). The accuracy and interference of the methods were evaluated with a urine chemistry control spiked with known quantities of PCM, uric acid, dopamine, ascorbic acid, caffeine, acetylsalicylic acid, tartrazine, sunset yellow, allure red, rutin, morin and metal ions. Finally, the novelty and usefulness of the composite were evaluated to quantify PCM in pharmaceutical dosage forms such as tablets, powders and syrups for children.

New approaches to identification and characterization of tioconazole in raw material and in pharmaceutical dosage forms / 药物分析学报

Tioconazole (TCZ), a broad-spectrum antifungal agent, has significant activity against Candida albicans and other Candida species, and therefore, it is indicated for the topical treatment of superficial mycoses. The main goal of this work is to report an exhaustive identification and characterization procedure to improve and facilitate the online quality control and continuous process monitoring of TCZ in bulk material and loaded in two different dosage forms: ovules and nail lacquer. The methodologies were based on thermal (differential scanning calorimetry (DSC), melting point, and thermogravimetry (TG)), spectroscopic (ultraviolet (UV), Raman, near infrared (NIR), infrared spectroscopy coupled to attenuated total reflectance (FTIR-ATR), and nuclear magnetic resonance (NMR)), microscopic and X-ray diffraction (XRD). The TCZ bulk powder showed a high crystallinity, as observed by XRD, with a particles size dis-tribution (3–95 mm) resolved by microscopic measurements. TCZ melting point (82.8℃) and a de-gradation peak centered at 297.8 ℃ were obtained by DSC and DTG, respectively. An unambiguous structure elucidation of TCZ was obtained by mono- and two- dimensional 1H and 13C NMR spectral data analysis. The FTIR-ATR, Raman and NIR spectra of both the raw material and the commercial products were analyzed and their characteristic bands were tabulated. The best methods for TCZ identification in ovules were DSC, TG, XRD, NIR and Raman, while NIR and FTIR-ATR were the most appropriate tech-niques to analyze it in the nail lacquer. DSC, TG, DRX, Raman, FTIR-ATR and NIR spectroscopy are effective techniques to be used in online process analysis, because they do not require sample preparation, and they are considerably sensitive to analyze complex samples.

Research Progress in Prevention and Treatment of Postoperative Abdominal Adhesions by Ligustrazine / 世界科学技术-中医药现代化

Ligustrazine is one of the active ingredients of chuanxiong. Modern medical research indicated that ligustrazine had the effect of improving microcirculation, anti-inflammatory, anti-fibrosis, which showed the potential function of ligustrazine in the prevention and treatment of postoperative abdominal adhesions. The basic theory of traditional Chinese medicine (TCM) also believed that ligustrazine had the unique double effect of regulating both qi and blood. Therefore, ligustrazin had broad research and application prospects in the prevention and treatment of postoperative abdominal adhesions. This article reviewed studies of ligustrazine in the prevention and treatment of postoperative abdominal adhesions in recent years from four aspects, which were theoretical basis, clinical application, mechanism research and pharmaceutical dosage forms. It identified the research status and advantages of ligustrazine in the prevention and treatment of postoperative abdominal adhesions. It also pointed out shortages in the clinical application, such as unstandardized medication, small sample size study and etc. There were insufficient deep and clear studies in the research of mechanism. In the aspect of pharmaceutical dosage forms, the thinking should be expanded with innovation. It will provide basis and direction for research and application in the future, in order to further elucidate mechanisms in the prevention and treatment of postoperative abdominal adhesions as well as provide theory basis, research thinking and methods for the real display of advantages in TCM.

Development and Validation of First Derivative Spectrophotometric Method for Quantification of Darunavir in Tablets.

Aims: Darunavir is widely used in HIV/AIDS therapy. It is a HIV protease inhibitor that has excellent efficacy against the virus. The aim of this study is to develop and validate an analytical method fast and free of interferences for determination of darunavir ethanolate as raw material and tablet dosage form. Methodology: As the formulation excipients show high interference in darunavir determination by a direct UV absorption measurement a derivative spectrophotometry was applied. A selective, easy and fast method was achieved employing simple and cheap instrumentation by using first-order derivative spectrophotometry. Results: The first-derivation of spectrum of the drug measured between 200 and 400 nm allowed identification of the analyte and showed absence of placebo interference. The assay was based on the absorbance at 276nm. The linear concentration range was established from 11 to 21 μg/mL. The intra-day and inter-day precision expressed as RSD was 0.06% and 3.75% respectively with mean recovery of 99.84%. Conclusion: The proposed analytical method is able to quantify darunavir as raw material and tablets and can be used routinely by any laboratory applying a spectrophotometer with a derivative accessory. The great difference of the method proposed here is that it proves to be free of placebo interferences as well as simple, fast and low cost.

RP-HPLC method development and validation for estimation of rivaroxaban in pharmaceutical dosage forms

Rivaroxaban, an anti-clotting medication, acts at a crucial point in the blood-clotting process and stops the formation of blood clots. In this study, RP-HPLC method was developed for the determination of rivaroxaban in tablets (Xarelto® (10 mg)). Phenomenex Luna 5 µm C18 100 Å LC Column (250 x 4.6 mm) was used at 40 ºC. Isocratic elution was performed with ACN:Water (55:45 v/v) mixture. The flow rate was 1.2 mL min-1 and UV detection was at 249 nm. Internal standard (Caffeine) and rivaroxaban were eluted within 2.21 and 3.37 minutes, respectively. The developed method was validated according to the ICH guidelines and found to be linear within the range 0.005 - 40.0 µg mL-1. The method was accurate, precise, robust and rapid. Thus, it was applied successfully for the quality control assay of rivaroxaban in tablet dosage form.

Rivaroxabana, fármaco anticoagulante, atua em um ponto crucial no processo de coagulação do sangue e impede a formação de coágulos sanguíneos. Neste estudo, desenvolveu-se método de RP-HPLC para a determinação de rivaroxabana em comprimidos (Xarelto ® (10 mg)). Utilizou-se coluna LC (250 x 4,6 mm) Phenomenex Luna C18 5 mm 100 Å a 40 ºC. Realizou-se eluição isocrática com ACN: água (55:45 v/v). O fluxo foi de 1,2 mL min-1 e a detecção de UV foi a 249 nm. Padrão interno (cafeína) e rivaroxabana eluíram em 2,21 e 3,37 minutos, respectivamente. O método desenvolvido foi validado de acordo com as diretrizes do ICH e mostrou-se linear na faixa 0,005-40,0 mg mL-1. O método foi exato, preciso, robusto e rápido. Assim, foi aplicado com êxito para o ensaio de controle de qualidade da Rivaroxabana na forma de comprimidos.

Functionality of innovative and generic celluloses in metronidazole formulations / Funcionalidade de celuloses inovadores e genéricos em formulações de metronidazol

The wide variety of excipients available calls for evaluation of their functionality, in this case of the pharmaceutical performance of microcrystalline celluloses and sodium cross-linked carboxymethylcelluloses from different sources. This evaluation includes parameters such as powder flow, compactibility, ejection pressure and dissolution from fast-release tablets as well as from floating granules and controlled-release tablets. In a previous study, the excipient Carmacel® presented better disintegration properties compared to Croscarmellose®. However, the evaluation showed better compactibility performance for Croscarmellose®. These characteristics were observed using pure excipients. Nevertheless, these advantages have not been confirmed in tests employing immediate-release or modified-release formulations containing metronidazole. Regarding microcrystalline celluloses, the present comparative evaluation between pure Alfacel ® types 101 and 102 and pure Avicel® types 101 and 102 showed better compactibility performance for the latter. However, for metronidazole formulations, this advantage was not evident in the innovative excipient. Notwithstanding, this study revealed better compactibility performance of microcrystalline cellulose type 101. In terms of powder flow properties, Avicel® and Alfacel® showed similar performance. However, the results revealed better powder flow employing microcrystalline cellulose type 102 for both excipients. Based on the results obtained, it can be concluded that the employment of innovative and generic excipients have both advantages and disadvantages. The observed differences however, tend to disappear as the excipients are diluted in a formulation, thereby equalizing their influence on product performance.

A variedade de excipientes disponível no mercado requer adequada seleção desses no que se refere à sua funcionalidade, como no caso de celuloses microcristalinas (Avicel® 101 e 102 e Alfacel® 101 e 102) e de carboximetilceluloses de sódio reticuladas (Croscarmellose® e Carmacel®), provenientes de diferentes fontes. Assim sendo, o desempenho farmacotécnico desses excipientes deve ser avaliado quanto ao fluxo e característica de compactação do pó, à pressão de expulsão do núcleo, ao perfil de dissolução de comprimidos de liberação imediata e modificada assim como de grânulos flutuantes. Em um trabalho anterior, o excipiente Carmacel® apresentou melhores propriedades de desintegração quando comparado ao Croscarmellose®, porém, no que se refere à característica de compactação a avaliação revelou melhor desempenho para o Croscarmellose®. Tais características foram observadas empregando apenas os excipientes. Porém, tais vantagens não foram confirmadas nos ensaios empregando as formulações de liberação imediata ou de liberação modificada contendo metronidazol. No que se refere às celuloses microcristalinas, a avaliação comparativa entre Alfacel® puro dos tipos 101 e 102 e Avicel® puro dos tipos 101 e 102 revelou melhor desempenho desse último quanto à característica de compactação, no entanto, para as formulações contendo metronidazol não foi possível demonstrar tal vantagem para o excipiente inovador. Porém, o estudo revelou melhor desempenho quanto à característica de compactação da celulose microcristalina do tipo 101. Quanto às propriedades relativas ao fluxo de pó, o Avicel® e o Alfacel® apresentaram desempenho semelhante. Porém, o estudo revelou melhor fluxo de pó no emprego da celulose microcristalina do tipo 102, para ambos os excipientes. Considerando os resultados obtidos, pode-se concluir que o emprego dos excipientes inovador e genérico apresentam vantagens e desvantagens. No entanto, as diferenças observadas tendem a desaparecer em função da diluição desses na formulação, equalizando, dessa forma, sua influência no desempenho do produto.