Simple and effective HPLC method development and its validation for Clindipine in human drug free plasma.

Simple and effective high performance liquid chromatographic (HPLC) method was developed for estimation of Clindipine in drug free human drug free blank plasma. The internal standard used as Nifidipine (IS). The current method was used protein precipitating extraction of Clindipine from blank plasma. Separation was achieved on reversed-phase c18 column (25cm × 4.6mm, 5µ) and the detection was monitored by UV detector at 260 nm. The optimized mobile phase was used acetonitrile: 5mM potassium dihydrogen orthophosphate (pH 4.5), in the ratio of 60:40% v/v at a flow rate of 1.0 ml/min. This linearity was achieved in this method range of 10.0-125.0 ng/ml with regression coefficient range is 0.99. The present method is suitable in terms of precise, accurate and specific during the study. The simplicity of the method allows for application in laboratories that lack sophisticated analytical instruments such as LC-MS/MS or GC-MS/MS that are complicated, costly and time consuming rather than a simple HPLC-UV method. The present method was successfully applied for pharmacokinetic studies.

Knowledge about the availability of the pharmacist in the Nuclear Medicine Department: A questionnaire-based study among health-care professionals.

OBJECTIVE: The objective of this study was to analyze the knowledge about the availability of the pharmacist in the nuclear medicine department among health-care professionals through a prospective cohort study. METHODS: A total of 741 health-care professionals participated in the study by answering 10 simple questions about the role of the pharmacist in the nuclear medicine department and the availability of pharmacist in the nuclear medicine department. An online questionnaire system was used to conduct the study, and participants were invited to participate through personal communications and by promoting the study through social websites including Facebook, LinkedIn and Google (including Gmail and Google+). The study was conducted between April 2013 and March 2014 using the http://www.freeonlinesurveys.com/Webserver. Finally, the data provided by 621 participants was analyzed. Group frequency analysis was performed using Statistical Package for the Social Sciences (SPSS) version 16 (SPSS Inc. USA). RESULTS: The participants were from Malaysia, India, Pakistan, Sri Lanka, Bangladesh, UAE and Nepal. In total, 312 (50.2%) female health-care professionals and 309 (49.8%) male health-care professionals participated in the study. Of the 621 participants, 390 were working in hospitals, and 231 were not working in hospitals. Of the participants who were working in hospitals, 57.6% were pharmacists. The proportion of study participants who were aware of nuclear pharmacists was 55.39%. Awareness about the role of the pharmacist in nuclear medicine was poor. CONCLUSION: The role of the pharmacist in a nuclear medicine unit needs to be highlighted and promoted among health-care professionals and hence that the nuclear medicine team can provide better pharmaceutical care.

Evaluation of sub-chronic toxic effects of petroleum ether, a laboratory solvent in Sprague-Dawley rats.

BACKGROUND: In general, organic solvents are inhibiting many physiological enzymes and alter the behavioural functions, but the available scientific knowledge on laboratory solvent induced organ specific toxins are very limited. Hence, the present study was planned to determine the sub-chronic toxic effects of petroleum ether (boiling point 40-60°C), a laboratory solvent in Sprague-Dawley (SD) rats. MATERIALS AND METHODS: The SD rats were divided into three different groups viz., control, low exposure petroleum ether (250 mg/kg; i.p.) and high exposure petroleum ether (500 mg/kg; i.p.) administered group. The animals were exposed with petroleum ether once daily for 2 weeks. Prior to the experiment and end of the experiment animals behaviour, locomotor and memory levels were monitored. Before initiating the study animals were trained for 2 weeks for its learning process and its memory levels were evaluated. Body weight (BW) analysis, locomotor activity, anxiogenic effect (elevated plus maze) and learning and memory (Morris water navigation task) were monitored at regular intervals. On 14(th) day of the experiment, few ml of blood sample was collected from all the experimental animals for estimation of biochemical parameters. At the end of the experiment, all the animals were sacrificed, and brain, liver, heart, and kidney were collected for biochemical and histopathological analysis. RESULTS: In rats, petroleum ether significantly altered the behavioural functions; reduced the locomotor activity, grip strength, learning and memory process; inhibited the regular body weight growth and caused anxiogenic effects. Dose-dependent organ specific toxicity with petroleum ether treated group was observed in brain, heart, lung, liver, and kidney. Extrapyramidal effects that include piloerection and cannibalism were also observed with petroleum ether administered group. These results suggested that the petroleum ether showed a significant decrease in central nervous system (CNS) activity, and it has dose-dependent toxicity on all vital organs. CONCLUSION: The dose-dependent CNS and organ specific toxicity was observed with sub-chronic administration of petroleum ether in SD rats.

Development and validation of an high-performance liquid chromatographic, and a ultraviolet spectrophotometric method for determination of Ambroxol hydrochloride in pharmaceutical preparations.

A high-performance liquid chromatographic (HPLC) and ultraviolet (UV) methods were developed and validated for the quantitative determination of Ambroxol hydrochloride (AMH) in pharmaceutical dosage form. HPLC was carried out by reversed phase (RP) technique on an RP-18 column with a mobile phase composed of acetonitrile and water (pH 3.5 adjusted with orthophosphoric acid [60:40, v/v]). UV method was performed with the λmax at 250 nm. Both the methods showed good linearity, reproducibility, and precision. No spectral or chromatographic interferences from the tablet excipients were found in UV and HPLC. The method was successfully applied to commercial tablets. Validation parameters such as linearity, precision, accuracy, and specificity were determined. The HPLC Limit of detection (LOD) and Limit of quantification (LOQ) for Ambroxol were found to be 1 and 5 ng/ml, respectively. The UV LOD and LOQ for Ambroxol were found to be 1 and 4 µg/ml, respectively. The results were statistically compared using one-way analysis of variance. The proposed economical method could be applicable for routine analysis of AMH and monitoring of the quality of marketed drugs.

Simple and sensitive method for the analysis of ketorolac in human plasma using high-performance liquid chromatography.

OBJECTIVE: To develop a simple and sensitive method of ketorolac in drug free human plasma using high-performance liquid chromatographic (HPLC). METHOD: Ketorolac from blank plasma was extracted using protein precipitation method. Trichloro acetic acid (10%) was used as a protein precipitating agent and the percentage of recovery was calculated by adding known volume of dexibuprofen as internal standard. The HPLC separation was achieved on reversed-phase C18 column and the separations were detection by Photodiode Array (PDA) detector at 306 nm. Acetonitrile and 5 mM ammonium acetate (pH 3.5), in the ratio of 60:40% v/v was used as mobile phase at the isocratic flow rate of 1.0 ml/min. The method was validated according to FDA Guidance for Industry. RESULT: The percentage of recovery of ketorolac was 93.7 ± 0.12 (mean ± SD; n = 5). The linearity was achieved in this method range of 10.0-125.0 ng/ml with regression coefficient range of 0.999. CONCLUSION: Ketorolac bioanalytical method was developed and validated according to FDA Guidance for Industry.

Pharmacokinetic-pharmacodynamic model of newly developed dexibuprofen sustained release formulations.

Pharmacokinetic-pharmacodynamic (PK-PD) modeling has emerged as a major tool in clinical pharmacology to optimize drug use by designing rational dosage forms and dosage regimes. Quantitative representation of the dose-concentration-response relationship should provide information for the prediction of the level of response to a certain level of drug dose. This paper describes the experimental details of the preformulation study, tablet manufacture, optimization, and bioanalytical methods for the estimation of dexibuprofen in human plasma. The hydrophilic matrix was prepared with xanthen gum with additives Avicel PH 102. The effect of the concentration of the polymer and different filler, on the in vitro drug release, was studied. Various pharmacokinetic parameters including AUC(0-t), AUC(0-∞), C(max), T(max), T(1/2), and elimination rate constant (K(el)) were determined from the plasma concentration of both formulations of test (dexibuprofen 300 mg) and reference (dexibuprofen 300 mg tablets). The merits of PK-PD in the development of dosage forms and how PK-PD model development necessitates the development of new drugs and bio analytical method development and validation are discussed. The objectives of the present study, namely, to develop and validate the methods to estimate the selected drugs in the biological fluids by HPLC, the development of in vitro dissolution methods, and PK-PD model development have been described.

Development of sustained release antipsychotic tablets using novel polysaccharide isolated from Delonix regia seeds and its pharmacokinetic studies.

A natural polysaccharide was isolated from the seeds of Delonix regia. The isolated polysaccharide could maintain aqueous equilibrium between the dosage form and the surrounding medium due to its massive competence of water absorption (80.72%) and swelling index (266.7%). The Scanning Electron Micrograph of a polysaccharide exhibits rough surface with pores and crevices, hence, the drug release will be retarded because of the drug particles entrapment in the pores and crevices. Further, the surface tension of polysaccharide is higher than that of water, which may facilitate sustained release of drugs from dosage forms. An antipsychotic drug, quetiapine fumarate has a short half-life of 6 h and administered multiple times per day. Hence the quetiapine fumarate oral sustained release tablets were formulated using this polysaccharide in the concentration of 5-30% to avoid the side effects and increase patient compliance. Dissolution of the developed tablets with 25% polysaccharide content showed a better release profile than the other batches (5-20%) at the end of 12 h. The strong matrix complex has low solubility in water, it does not dissolve rapidly and the drug continues to diffuse through the gel layer at a consistent rate. Drug release from the matrix tablets follows matrix type except F-4 and F-5 which follow first order and Hix.crow type. The bioavailability study was carried out using healthy male New Zealand white rabbits that show the AUC(0-inf) value for developed SR tablets is 1.44 times higher than the reference thus, indicating more efficient and sustained drug delivery capable of maintaining plasma drug levels better.

Development and Validation of a HPLC and an UV Spectrophotometric Methods for Determination of Dexibuprofen in Pharmaceutical Preparations.

A high-performance liquid chromatographic (HPLC) and a ultraviolet (UV) methods were developed and validated for the quantitative determination of Dexibuprofen (DI) in pharmaceutical dosage form. HPLC was carried out by reversed phase technique on a RP-18 column with a mobile phase composed of acetonitrile and 0.5% triethylamine (pH 7.5 adjusted with orthophosphoric acid (30 : 70, v/v)). UV method was performed with the λ max at 222.0 nm. Both the methods showed good linearity, reproducibility and precision. No spectral or chromatographic interferences from the tablet excipients were found in UV and HPLC. The method was successfully applied to commercial DEXIFEN tablets. Validation parameters such as linearity, precision, accuracy, and specificity were determined. The proposed method could be applicable for routine analysis of DI and monitoring of the quality of marketed drugs.

Bilayer tablets of atorvastatin calcium and nicotinic acid: formulation and evaluation.

The objective of the study is to formulate bilayer tablets consisting of atorvastatin calcium (AT) as an immediate release layer and nicotinic acid (NA) as an extended release layer. The immediate release layer was prepared using super disintegrant croscarmellose sodium and extended release layer using hydroxypropylmethyl cellulose (HPMC K100M). Both the matrix and bilayer tablets were evaluated for hardness, friability, weight variation, thickness, and drug content uniformity and subjected to in vitro drug release studies. The amount of AT and NA released at different time intervals were estimated by HPLC method. The bilayer tablets showed no significant change either in physical appearance, drug content or in dissolution pattern after storing at 40 degrees C/75% relative humiding (RH) for 3 months. The release of the drug from the tablet was influenced by the polymer content and it was much evident from thermogravimetry/differential thermal analysis (TG/DTA) analysis. The results indicated that the bilayer tablets could be a potential dosage form for delivering AT and NA.