心宁缓释片的质量标准研究

目的:建立心宁缓释片的质量标准控制方法.方法:采用TLC对丹参提取物、B草SFE-CO2萃取物进行定性鉴别,采用紫外分光光度法对制剂中总酚酸与总生物碱进行含量测定,采用HPLC法测定制剂中丹酚酸B、HJJ的含量及其释放度.结果:薄层色谱图斑点清晰,具有专属性.总丹酚酸、总生物碱、丹酚酸B、HJJ分别在2.5-25μg/mL、1.6-16μg/mL、0.88-11μg、0.08-0.8μg范围内线性关系良好,相关系数R分别为0.999 9、0.999 8、0.999 5、0.999 9,其平均回收率分别为98.26%、99.34%、97.34%、97.86%,RSD分别为2.1%、0.58%、0.95%、1.53%,累计释放率在2 h时约为25%、8 h时约75%、12 h时达94%以上.结论:该方法能准确可靠地进行定性、定量检测,能有效地控制心宁缓释片的质量.     

Stability studies of alprazolam tablets: effects of chemical interactions with some excipients in pharmaceutical solid preparations

An HPLC method was developed to determine the stability of alprazolam (AL) as a pure drug and in monodrug pharmaceutical tablets. The main degradation product of AL tablets was isolated and fully characterized as triazolaminoquinoleine (TAQ). For a quantitative evaluation of the excipient effects in the pharmaceutical formulations, a 2^k fractionated factorial design was applied in the preparation of the different samples. The kinetic of degradation of AL in each formulation was followed by UV spectrophotometry. It was found that excipients like CMC and magnesium stearate favour degradation, while the rate of the reaction is decreased when lactose and starch were used as excipients. A mechanism for the interactions of AL with some excipients is postulated that explains the observed results. Copyright © 2009 John Wiley & Sons, Ltd.     

卡托普利缓释片释放过程的灰色数学模型

目的:用灰色理论研究卡托普利缓释片的体外释放过程.方法:采用羧甲基纤维素钠为骨架材料制备缓释片,通过体外释放试验,根据灰色数学模型,预测卡托普利缓释片的体外释放过程.结果:预测值与实测值的平均绝对误差E为0.532,平均相对误差为1.059%.结论:为卡托普利缓释片的临床合理化用药提供了理论依据.     

Determination of iodine anion in dried kelp and iodized throat tablets by reversed-phase ion-pair liquid chromatography with direct UV detection

Summary In this paper, the amount of iodine anion in dried kelp and iodized throat tablets was determined by reversed-phase ion-pair chromatography. A 300×4 mm I.D. columns packed with -Bondapak-C18 (5 m) was used and distilled water containing 10 mmol/l trimethylphenyl ammonium bromide was used as the eluent. UV detection at 231 nm was selected to monitor the iodine anion.     

In vivo Antimalarial Activity of Andrographis Paniculata Tablets

The formulation of three phytopharmaceutical products of Andrographispaniculata fractions (AP fraction A and B) containing diterpene lactones as an active substance were developed and their antimalarial activities against Plasmodium bergheihas been examined. In vivo antimalarial assay on P. berghei infected mice was carried out by oral administration,twice a dayfor four consecutive days of the AP fractions product, which were Tablet I: wet granulated formula of AP fraction A; Tablet II: wet granulated formula of AP fraction B; Tablet III: solid dispersion formula of AP fraction B.. The results revealed that three phytopharmaceutical products of A.paniculata were inhibited parasite's growth with inhibition range of 70.15% to 80.35%. There was no significant difference of antimalarial activities between Tablet II and III, meanwhile there was significant difference among Tablet I with Tablet II and Tablet III.It was concluded that antimalarial activity depending on raw material form of A. paniculata active substance.     

Characterization of factors affecting the release of low-solubility drug from prolonged release tablets

Diclofenac sodium (2-[(2,6-dichlorophenyl)amino]benzeneacetic acid monosodium salt) was investigated as a low-solubility drug and Naklofen^® retard prolonged release tablets, containing 100 mg of diclofenac sodium as a prolonged release lipophilic matrix system using factorial design approach. First, the solubility characteristics of diclofenac sodium in aqueous media with various ionic strengths, ionic compositions and pH in the range of 1-8 were determined. The obtained results showed that the solubility of diclofenac sodium depends mainly on pH of the aqueous medium and less on the composition and ionic strength of the medium. Next, the estimation of the effects of six different factors (type of the dissolution apparatus, rotation speeds of the stirring elements, pH, ionic strengths of dissolution medium, the applied salt, and the producer of the on-line connected dissolution apparatus and UV spectrophotometer) on the release of diclofenac sodium, using the two-level six-factorial design was investigated. It was found that rotation speeds of the stirring elements, pH, and ionic strengths of the dissolution medium have a significant impact on the drug release and should be further followed in future drug release analyses. The advantages of the factorial design approach are obvious in this work. It is a very economic way of obtaining the maximum amount of information in a short period of time, especially in the case of prolonged release formulations where each experiment requires at least 24 h.     

Determination of ticagrelol in rat plasma and tablets by micellar electrokinetic chromatography coupled with large volume sample stacking: Application to a pharmacokinetic study

A method using micellar electrokinetic chromatography coupled with large-volume sample stacking for the determination of ticagrelol was developed and validated. The analysis was performed in a fused silica capillary (41.5 cm effective length, 50 μm diameter) with ultraviolet detection at 195 nm. The background electrolytes were 30 mM phosphate buffer of pH 3.0 with 120 mM sodium dodecylsulfate and 10 % (v/v) acetonitrile (120 s X 50 mbar; 20°C; -18 kV) and 30 mM borate buffer of pH 8.5 with 75 mM sodium dodecylsulfate (120 s X 50 mbar; 20°C; 25 kV); under acidic and alkaline conditions, respectively. The method was found to be reliable with respect to specificity, linearity of the calibration line (R² > 0.99), repeatability (relative standard deviation 2.56%–3.34%), and accuracy (recovery in the range 101.21%–102.67%). The limits of detection and quantitation were 0.032, 0.071, and 0.087, 0.188 μg/mL, respectively. The method was successfully applied for the determination of ticagrelol concentrations in rat plasma and tablets with good recoveries and reproducibility. The presented method proved to be suitable for monitoring ticagrelor in rat plasma.     

An HPLC Procedure for the Analysis of Furosemide in Pharmaceuticals-Analysis of Furosemide Tablets and Furosemide Injection

Abstract

A simple and specific procedure was developed for the analysis of furosemide from tablets and injections. The procedure consists of extracting furosemide into aqueous sodium hydroxide, addition of the internal standard, appropriate dilution and injection onto a u Bondapak C₁₈ reversed phase column. The mobile phase consisted of a solvent containing acetonitrile and aqueous sodium acetate and the eluate was monitored by either U.V. absorption or spectrofluorimetry. A standard linear calibration curve was obtained for direct standard solutions containing 75 ng to 500 ng on column. This procedure was successfully used to analyze furosemide tablets (individual assay) and injections.     

Selective Spectrophotometric Determination of Oxyphenbutazone Using a Chelate Forming Reaction

Abstract

A selective spectrophotometric method for the determination of oxyphenbutazone is described. The method is based on nitrosation reaction and simultaneous formation of copper(II) or cobalt (II) chelate of the nitrosoderivative. The formed chelates are extractable with organic solvents giving yellow solutions whose absorbance are proportional to the concentration of oxyphenbutazone. In addition, the chelate extracts, upon treatment with diethyldithiocarbomate develop an additional indirect method of high selectivity for determining oxyphenbutazone. The developed methods are highly accurate and comparable with an official method.     

D1-Differential Potentiometric and 1H-NMR Spectrometric Determinations of Ketoconazole and its Formulations

Abstract

Two rapid and direct quantitative assays have been investigated for ketoconazole alone and in tablet form. the first one is a non-aqueous potentiometric titration in which the equivalence point has been located graphically using its distinct and sharp D₁differential (peak-shape) potentiograph. the second is based on ₁H-NMR spectrometry and involves the integration of the methyl protons-signal of ketoconazole (at 2.07 δ) relative to that of benzocaine (at 1.30 δ) which is used as internal standard. the obtained results were in good agreement with regard to accuracy, precision as well as sensitivity and reproducibility. However, by comparison with the official USP procedure, the two methods were significantly more accurate and more sensitive. the validity of the two methods were confirmed using the authentic addition technique.