Safila Naveed

RP-HPLC Method for Simultaneous Determination of Captopril and Diuretics: Application in Pharmaceutical Dosage Forms and Human Serum

An isocratic reversed phase high-performance liquid chromatographic (RP-HPLC) method has been developed for the simultaneous determination of captopril and diuretics (furosemide and hydrochlorothiazide) in API, dosage formulations and human serum. Chromatographic separation was achieved on Purospher Start C18 (250 mm x 4.6 mm, 5 μm) and Hypersil ODS C18 (150×4.6mm, 5micron) columns using mobile phase, methanol: water (70:30 v/v) adjusted to pH 3.0 via phosphoric acid 85% having flow rate of 1.0 mL min -1 at ambient temperature with detector set at 225 nm. Calibration curves were linear over range of 5-25 μg mL -1 with a correlation coefficient ± 0.999. LOD and LOQ were in the ranges of 0.4-2.3 μg mL -1 . Intra and inter-run precision and accuracy results were 98.0 to 102%.

Analytical Determination of Lisinopril Using UV Spectrophotometer and HPLC: An Overview

Present review article determine the analytical methods for the quantitative determinations of lisinopril (ACE Inhibitor) by UV spectrophotometery and High-Performance Liquid chromatography. Pharmaceutical analysis of lisinopril requires effective analytical procedures for QC quality control analysis in Pharmaceuticals dosage formulations and human serum. An extensive survey for determination of LSP compiled from the research articles published in various pharmaceutical and analytical chemistry Journals. This appraisal illustrate that majority of the HPLC methods reviewed are based on the quantitative analysis of drug in Active Pharmaceutical ingredients (API), formulations, biological fluids such as serum and plasma and they are appropriate for therapeutic monitoring of drug, for pharmacokinetic purpose.

DEGRADATION STUDY OF FIVE DIFFERENT B RANDS OF CIPROFLOXACIN USING UV VISIBLE SPECTROPHOTOMETER AND THEIR COMPARATIVE STUDY

Degradation studies help to anticipate the future stability issue the drug product may undergo, and provide useful information for both formulation and stability. We explored the degree of degradati on in five dif ferent brands of C iprofloxacin tablet, with the purpose to determine the most stable brand out of the five. 500 ppm and 250 ppm samples of each brand were prepared to observ e the effect of time, acid (0.1N HCl) and base (0.1 N NaOH). Their absorbance was re corded using a Shimadzu UV - Visible spectrophotometer at 2 71.4 nm. The results suggest tha t out of the five brands, c yrocin possessed the highest stability and degraded the least.

RP-HPLC Method for the Simultaneous Determination of Captopril andH2-Receptor Antagonist: Application to Interaction Studies

Rapid, sensitive, simple and accurate high-performance liquid chromatographic (HPLC) method is developed and validated for the simultaneous determination of captopril with H2 receptor antagonists as cimetidine, ranitidine and famotidine. Captopril was separated from H2 receptor antagonist using pre packed Purospher star C18 (5 μm, 25×0.46 cm) column methanol: water (60:40 v/v) were used as the mobile phase, pH 3.0 ± 0.02 was adjusted by orthophosphoric acid. The flow rate was 0.8 mLmin-1 at ambient temperature, diluent was 50:50 methanol water while UV detection was performed at 225 nm. The retention time for captopril was found to be 5.2 minute, for ranitidine and famotidine 2.5 minute and cimetidine 2.7 minute. Each drug showed a good resolution from captopril. In vitro interaction studies of captopril with commonly administered H2 receptor antagonists i.e. cimetidine, ranitidine and famotidine were carried out at 37°C using above validated method. These studies clearly indicated that H2-receptor antagonists bind to captopril causing drastic changes in the availability of the drug.

Monitoring of in vitro interaction studies of enalapril with hypoglycemic agents by LC-UV

The coadministration of antihypertensive and antidiabetic drugs is common, as both of these ailments are synergistic to each other and often occur together. In the present paper, we describe in vitro drug interactions of enalapril, an antihypertensive drug, with the hypoglycemic agents, metformin, glibenclamide, and glimepiride. These studies were carried out using an isocratic reversed phase high-performance liquid chromatographic method using a C18 column with ultraviolet detection at 230 nm. The system was operated at room temperature using a mobile phase consisting of methanol:water (70:30) adjusted to pH 2.5 with o-phosphoric acid with a flow rate of 1 mL minute −1 . The assay was reproducible, linear (concentration range of 2.5-100 µg mL −1 ) with a correlation coefficient of 0.9999 and an accuracy rate of 98%-102%. The results from the reversed phase high-performance liquid chromatographic method clearly indicated that the availability of enalapril was unaffected by the simultaneous administration of hypoglycemic agents. Hence, the two drugs can be safely administered with one another.

Development and Validation of a Simple and Efficient RPLC Method for Analysis of Captopril, Metformin, Pioglitazone and Glibenclamide in API, Formulations and Human Serum

The association between the use of ACE inhibitors and the incidence of hypoglycemia is controversial. A recent study reported that 14% of all hospital admissions for hypoglycemia might be attributable to ACE inhibitors. In this paper, a novel, precise, specific, accurate and rapid reversed-phase high performance liquid chromatographic method was developed, optimized and validated for determining captopril and hypoglycemic (metformin, pioglit azone and glibenc lamide) in bulk, pharmaceutical formulations and human serum with the best chromatographic peak resolution, reduced run time and low cost of analysis. The method was validated according to the US Food and Drug Administration (FDA) and ICH guidelines for the parameters: specificity, stability, limits of detection (LLOD), limits of quantification (LLOQ), linearity, accuracy, precision and recovery. This method showed the best resolution by using Hypersil ODS,C18 (150×4.6 mm, 5 micron) column using mobile phase, methanol: water (70: 30 v/v) adjusted to pH 3 via ortho phosphoric acid 85% with flow rate of 1 mLmin -1 at ambient temperature and wavelength of 230 nm. The signal-to-noise ratio (S/N) was employed as a quality measurement. This tool permits to establish the influence of some selected factors (methanol: water ratio, pH, and flow rate) on two responses (peak areas and retention time). The LLOD and LLOQ values for CAP, MET, PGL and GLB were found to be 2.3, 1.5, 2.3 and 2.3 and 0.7, 0.4, 0.7, and 0.7 μgmL-1 respectively. Calibration curves were linear in the concentration range of 2.5-100 μgmL -1 for hypoglycemic and captopril with regression coefficient (r 2 ) value of 0.999 for all drugs. The data for accuracy, precision and recovery were within the FDA limits. Intra ad inter-day precision and accuracy results were 98.0 to 102%. Retention time for captopril was found to be 3.3 minute and for metformin, pioglitazone and glibenclamide 2.4, 2.8, 7.2 minutes respectively. Proposed method was selective, precise and accurate short time analysis therefore can be used for routine, quality control and clinical study. This is the first full report of a method for the simultaneous determination of these four drugs: captopril , metformin, pioglita zone and glibenclamide in API, formulations and serum. The newly developed method is useful for future routine analysis of these drugs and could be used in therapeutic drug monitoring and adherence to medicine studies, which would be helpful in decision making regarding treatment change in combination therapies.

HPLC-UV Method for the Determination of Enalapril in Bulk, Pharmaceutical Formulations and Serum

A simple reversed phase HPLC method have been successfully developed and validated for the quantitative determination of enalapril maleate (ENP) in bulk material, pharmaceutical formulation and serum. Purospher Start C 18 (250 cm x 4.6 mm, 5 μm) and Hypersil, ODS columns were used. The mobile phase, methanol-acetonitrile-water (70:30v/v pH 3.5 adjusted by phosphoric acid), was delivered at a flow rate of 1 mLmin -1 , eluent was monitored using UV detector at 215 nm. The proposed method is specific, accurate (99-102%), precise (intra-day and inter-day variation 0.07-1.25%) and linearity (R 2 >0.999) within the desired range 2.5-100 μgmL -1 concentration. The detection limit and quantification 3.9 ngmL -1 and 12 ngmL -1 respectively. The anticipated method is applicable to routine analysis of ENP in pharmaceutical formulations as well as in human serum samples.

Knowledge and Attitude about Crimean Congo Hemorrhagic Fever (CCHF) amongst Local Residents of Karachi, Pakistan

Background: Crimean Congo Hemorrhagic Fever (CCHF), a tick-borne disease has been in the news with reports of its outbreak in Pakistan. Pakistan is considered as an endemic country for CCHF during last two decades . Humans get this infection after a bite of an infected tick or from one infected human to another by contact with infectious blood or body fluids. Aim: To assess the level of knowledge regarding Crimean Congo Hemorrhagic Fever (CCHF) among the local residence of Karachi, Pakistan. Method: This questionnaire based cross-sectional survey was conducted among the local residence of Karachi, Pakistan. The questionnaire was composed of 20 questions. The questionnaire included demographic information with their designation and knowledge level regarding sources, transmission, symptoms, prevention and treatment of Crimean Congo Hemorrhagic Fever (CCHF). Result: A total of 150 respondents interviewed in the survey. Sufficient knowledge about CCHF was not found in (23%) of the respondent participants. Literate individuals (71%) were relatively better knowledge about CCHF as compared to the illiterate people (29%). Television and internet (50%) were considered as the most important and useful source of information on the disease. Conclusion: This study revealed that the knowledge level of Karachi citizens about CCHF was insufficient. The need to educate the public about CCHF and the ticks is at an alarming level. As this disease can cause fatalities if the general community are not be informed and trained adequately. TV/radio broadcasts may be sufficient for the general public, but specialized educational programs and workshops are recommended for health workers and veterinary staffs.

In vivo interaction studies of lisinopril with flurbiprofen and ibuprofen on carrageenan induced inflammation

D recent years, a sudden rise in interest for biosimilar molecules by large pharmaceuticals has been evident due to two major factors i.e., larger application of biosimilars strategy to control escalating health-care cost and impending expiration of patents of popular blockbusters. Analytical strategy adopted for these molecules, widely differs from that of small molecules, due to inherent variations in living systems involved during manufacturing process and large size of biomolecules. Considering these facts, regulators have also emphasized multidimensional (structural, cellular potency and similar clinical efficacy) approach for their market approvals.Analytical strategy adopted for qualification and quantitation of P-38 (Mol. Wt. 44 kDa) and mAb (Mol.Wt. 141 kDa) molecules, demonstrate a systematic approach towards such applications. Qualitative analysis included BioConfirm set-up and acquisition of Q1 spectrum for molecules. Mol. Wt. was confirmed through deconvoluted spectrum approach and had a good agreement with theoretical reference. Phosphogluconoylation (for P-38) and glycans presence (for mAb) were manifested in decisions for quantitation strategy.Selection of multiple qualifier ions (m/z 3156.6988 and 2736.0254) for single quantifier ion (m/z 3087.5633) was adopted for establishing linearity from 15 to 300 nanogram for P-38 (top-down approach). To demonstrate bottom-up approach; mAb was digested with LysC enzyme and extracts were analyzed to establish a linearity for range of 1 to 4000 microgram range using four quantifier ions (m/z 495.7553, 481.7634, 321.5115 and 288.1718). Above strategy provides a clear rational approach for discovery researches to begin and implement analytical instrumentation approach towards large biological therapeutics quantitation.B has facilitated the discovery of treatments for some of the most severe diseases known to man – worldwide. Now days in market, patients have access to many biotechnology drugs and vaccines, and medical science is working to grow that number every day. Biologic medicines are made in living organisms to produce proteins to treat various diseases, often by genetically modifying cell constructs or cell lines. When exclusive rights like patents for the first generation of approved biopharmaceuticals got either expired or are about to expire, the market is opening for generic versions, referred to as ‘biosimilars’ (European Union) or ‘follow-on protein products’ (United States). These are also called as similar biological medicines. Some of these are already on the market in Europe. Biosimilar medicine is similar to biological medicine which has already been authorized as the ‘biological reference medicine’. The active ingredients of both biosimilar medicine and biological medicine are similar and are used in general at the same dose to treat the same disease. Since biosimilar and biological reference medicines are similar but not identical, so the name, appearance and packaging of a biosimilar medicine differ to those of the biological reference medicine. A biosimilar manufacturer must commence pre-clinical and clinical studies so as to present pertinent data which establishes the quality, safety and efficacy of the product, as well as its similarity with the reference product. Biosimilars are still new and emerging market. Regulatory guidelines and standards are still being developed in some countries and they are constantly evolving as technology develops.In vivo interaction studies of ACE inhibitor (captopril) was carried out with commonly used NSAIDs (flurbiprofen and ibuprofen) in carrageenan induced inflammation (CII) rats to check the anti-inflammatory response of NSAIDs with captopril and alone. In our study the altered anti-inflammatory response was observe for NSAIDs when given simultaneously with captopril by comparing decrease in paw size (edema). Results were expressed in% reduction in paw size for every hour and were calculated for edema rate and percentage reduction using the formula, Edema rate (E%)=VT – VO/VO * 100 Where, VO=Rat’s hind paw volume before 1% Carrageenan administration and VT=Rat’s hind paw volume at t hour. Percentage reduction (R%)=E C – E T \ E C *100 Where, E C =Edema rate of control group and E T =Edema rate of test compound at t hour. Tukey’s post-hoc test was conducted to determine group means differences taking significant level p<0.05 and p<0.005 highly significant. It has been observed while comparing the anti-inflammatory response of commonly used NSAIDs alone and in combination with captopril that the activity of NSAIDs was enhanced by the addition of captopril as% reduction got higher and edema rate decreased. The synergistic effects of captopril with flurbiprofen and ibuprofen were observed on reduction of inflammation.

Knowledge of Amyotrophic Lateral Sclerosis (ALS) in Pharmacy Students

A motor neuron disease, known as (ALS) Amyotrophic lateral sclerosis in which neuronal muscles becomes atrophic. There is a loss of control of the brain on voluntary muscles occurs. Signs and symptoms of the disease vary according to the condition of a patient. There is no specific diagnostic test and treatment yet for this disease. Our survey aimed to find out its awareness among the university students of Karachi, Pakistan. Data of 50 university students was collected and analyzed. A cross-sectional and random method was used to collect data. Different questions were asked the awareness regarding the disease among university students. Only 10% students have basic information regarding this disease. 2% students have information about the signs and symptoms, 2% students have information about the diagnosis, and 4% students have information regarding the treatment strategies of this motor neuron disease, Amyotrophic lateral sclerosis (ALS) in our survey. This survey proved that there is no awareness about ALS or only a negligible awareness among university students in the Karachi city. Even there were many students who heard this term “Amyotrophic lateral sclerosis (ALS)” first time in their lives.