Current Issue : July - September Volume : 2011 Issue Number : 3 Articles : 22 Articles
The World Health Organization has called for an effort to eliminate Lymphatic Filariasis (LF) around the world. In regions where the disease is endemic, local production and distribution of medicated salt dosed with diethylcarbamazine (DEC) has been an effective method for eradicating LF. A partner of the Notre Dame Haiti program, Group SPES in Port-au-Prince, Haiti, produces a medicated salt called Bon Sel. Coarse salt is pre-washed and sprayed with a solution of DEC citrate and potassium iodate. Iodine levels are routinely monitored on site by a titrimetric method. However, the factory had no method for monitoring DEC. Critical analytical issues include 1) determining whether the amount of DEC in each lot of Bon Sel is within safe and therapeutically useful limits, 2) monitoring variability within and between production runs, and 3) determining the effect of a common local practice (washing salt before use) on the availability of DEC. This paper describes a novel titrimetric method for analysis of DEC citrate in medicated salt. The analysis needs no electrical power and requires only a balance, volumetric glassware, and burets that most salt production programs have on hand for monitoring iodine levels. The staff of the factory used this analysis method on site to detect underloading of DEC on the salt by their sprayer and to test a process change that fixed the problem....
Ultra Performance Liquid Chromatography (UPLC) is a relatively new technique giving new possibilities in liquid chromatography, especially concerning decrease of time and solvent consumption. UPLC Chromatographic system is designed in a special way to withstand high system back-pressures. Special analytical columns UPLC BEH C18 packed with 1.7 μm particles are used in connection with this system. The quality control analyses of various pharmaceutical formulations are transferred from HPLC to UPLC system. The UPLC system allows shortening analysis time up to nine times and three times comparing to the conventional system using 5 μm and 3 μm particle packed analytical columns respectively. ACQUITY Ultra Performance LC Systems take advantage of technological strides made in particle chemistry performance, system optimization, detector design, and data processing and control. When taken together, these achievements have created a step-function improvement in chromatographic performance. Defined as UPLC, this new category of analytical separation science retains the practicality and principles of HPLC while increasing the overall interlaced attributes of speed, sensitivity, and resolution....
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The hydro-distilled medicinal fixed oil of the Calotropis gigantea (Asclepiadaceae) commonly called as Rui was investigated by GC-MS. Six compounds from Calotropis gigantea was characterized. Methyl Octadecanoate (Steric acid 55.95%), Hexadecanoic acid (Palmitic acid 30.06%), Tetradecanoic acid (Myristic acid 8.17%) were found to be the major compounds of Calotropis gigantea while Heptadecanoic acid (2.41%), Ethyl linoleate (1.38%),9, 10-Octadecanoic acid (Linoleic acid 4.03%) were found to be minor compounds. The purpose of the present study was to examine the fatty acid composition of seed oil....
This study was carried out to analyze the active constituents present in leaf of Passiflora incarnata L. (Passfloraceae). Eleven compounds in ethanolic extract are identified by Gas Chromatography -Mass spectrometry(GC-MS) analysis. Hexanedioic acid, bis(2-ethlhexyl) ester (36.29%)was a prevailing compound in alcoholic extract. This is the first report of identification of active constituents from leaf of Passiflora incarnata by GC-MS....
The present work describes a validated reverse phase high performance liquid chromatographic method for simultaneous estimation of Spironolactone and Torsemide in tablet dosage form. The separations were achieved using Inertsil C8 column, 10µm, {250 × 4.6 mm (i.d.)} with a mobile phase consisting of Methanol: Acetonitrile: 0.05M NaH2PO4 buffer, (40:30:30%v/v/v)) pH 7.1 is adjusted with triethylamine, at the flow rate of 1ml/min, detection was carried at 257nm using a variable wavelength UV-1575 detector. The retention time for Torsemide was about 3.67 minutes and for Spironolactone was about 6.56 minutes. The linearity for Torsemide 02-20 g/ml and Spironolactone in the range of 10-100 µg/ml, respectively. The Proposed method was found to be accurate, precise, simple, specific and rapid can be used for simultaneous estimation of Spironolactone and Torsemide in tablet formulation....
Healthcare products must be sterilized before shipping. During sterilization the quality of the products must be maintained. Polysulfone (PS) and polycarbonate (PC) are often used as materials for medical devices. It has been observed that compounds inhibiting bacterial growth are produced when PS or PC are sterilized by autoclaving or by use of ozone gas, especially when ozone gas is used to sterilize PS. This study was conducted to identify the compounds inhibiting bacterial growth. An ethanol extract of the sterilized PS or PC was analyzed by liquid chromatography-moss spectrometry-UV photodiode array (210-350 nm) for identification and determination of the inhibitors. Bisphenol A, 4,4�-dihydroxydiphenyl sulfone (bisphenol S), and 4-chloro-4�-hydroxydiphenyl sulfone were identified in PS sterilized with ozone gas. Bisphenol A was also identified in PC sterilized with ozone gas. Bisphenol A was not a major inhibitor of bacterial growth because the extent of inhibition did not correlate with the amount of bisphenol A produced. Inhibition by 4-chloro-4�-hydroxydiphenyl sulfone was greater than by bisphenol S and correlated with the amount produced; the major inhibitor might therefore be 4-chloro-4�-hydroxydiphenyl sulfone. The synergistic effect of bisphenol S and 4-chloro-4�-hydroxydiphenyl sulfone might be a more realistic measure of the exact amount of inhibition...
Sodium lauryl sulphte(SLS) is a sodium salt of sulphuric acid mono dodecyl ester. It is mainly used as surface-active agent in detergents/or wetting agent in cosmetics, food, pharmaceuticals and different toiletry preparations.It produces adverse reactions when used in higher concentrations as in case of cosmetics (e.g. shampoos). Its severetoxic effects including irritation to the skin, eyes, mucous membranes, upper respiratory tract, and stomach. Repeated, prolonged contact can cause drying and cracking of the skin.This shows the need to determine SLS from shampoos- the most widely used cosmetics now-a-days. The determination of SLS various methods was use such as: potentiometric, Spectrophotometric using colorimerty, uv-visible spectrophotometer, Thin layer chromatography, Gas chromatography, HPLC, LC-MS, capillary zone electrophoresis. This review is about different methods for the detection of such a critical ingredient - sodium lauryl sulphate...
Retrospective validation should be performed in order to validate a well established process which has not been validated before or if validated already, then to re-check and reassure the validation work. Retrospective validation can also be performed to keep an eye on a track record and consistency in the performance of a process. A retrospective validation study report on applying control charts and trend analysis method; had proved that a manufacturing process under consideration was consistent throughout selected retrospective validation batches. Control charts showed that all process parameters were well within the control limits and also the values for few of the selected process parameters doesn’t show deviation out of three sigma (3σ) level of control. Process capability Indices (Cp, Cpk) were having values very near to that of 1.33, which is a benchmark value of capability indices accepted by many companies around the world. Thus, with Cp and Cpk values of 1.43 and 1.08 & the sigma level achieved was of four sigma (4 σ), that means process can be capable of producing process yield of up to approximately 99.99 % or process can show a process fallout of approximately 63 PPM....
A simple, precise, accurate, reproducible, robust HPLC method was developed for the estimation of Rizatritan benzoate from oro-dispersible tablet dosage form .The method was validated as per ICH and FDA guidelines. Analysis of the drug was performed on Phenomenex Luna C18 (250mm×4.6 mm, 5µ) column, in an isocratic mode employing pH 6.5 phosphate buffer, Acetonitrile and methanol (87:7.8:5.2) as the mobile phase. UV-Visible detector at 225nm was found to be suitable for detection. Linearity was observed in the range of 5-60 µg/ml. Recovery values were found to be 98.2-100.4% .The % RSD values for method precision and system precision were found to be 0.22 and 0.20 respectively. Limit of detection and limit of quantification of the method were found to be0.0014 µg/ml and 0.0043µg/ml respectively....
GLP address all aspects of a laboratory study intended for submission to a regulatory agency and the intent of regulation is to assure quality and integrity of safety data. (GCP) is an international ethical and scientific quality standard for the design, conduct, Performance, monitoring, auditing, recording, analyses and reporting of clinical trials. It also serves to protect the rights, integrity and confidentiality of trial subjects. It is very important to understand the background of the formation of the ICH-GCP guidelines as this, in itself, explains the reasons and the need for doing so. In this paper, we addressed the historical background and the events that led up to the formation of these guidelines. Today, the ICH-GCP guidelines are used in clinical trials throughout the globe with the main aim of protecting and preserving human rights. While GCP is an international quality standard that defines standard which governments can transpose into regulations for clinical trials involving human subjects. The manuscripts describe all aspect of GLP and GCP guideline include protection of animal and human rights respectively as a subject in preclinical and clinical trial and provides assurance of safety and efficacy of newly developed compounds....
The pharmaceutical industry is in rapid transition from a supply-driven market to a demand and service-driven market where manufacturing efficiency and responsiveness will play a critical role in future success. Pharmaceutical manufacturers generously allocate funds to research and marketing, but they as a whole lags behind other automated industries in one key aspect: manufacturing quality analysis. To overcome this there is growing enthusiasm in the industry for the many potential gains offered by process analytical technology, a new FDA initiative that aims to foster improvements in manufacturing efficiency and quality analysis. Pharma Industry is facing growing demands for increased productivity and reduced manufacturing costs and also has to meet the evolving need for higher quality standards and higher drug expectations The regulatory area appears to be rapidly evolving, with PAT initiative to be the first major change in the GMP's in over 25 years that is based on increased scientific understanding and less on an empirical based approach. The underlying premise of process analytical technology is that quality cannot be tested into products; instead it should be built-in or should be by design. Along with benefits there are numerous technical, cultural, organization and regulatory hurdles on the PAT path....
A simple, precise, specific and reproducible HPTLC method is described for the simultaneous quantification of Atorvastatin calcium, Fenofibrate and Ezetimibe in a ternary mixture. The method was based on separation of three drugs on Merck aluminium plates precoated with silica gel 60 F254 using Toluene: methanol: acetone: triethylamine (7:2:1:0.2 v/v) as mobile phase. Quantitative analysis was performed by densitometric scanning at 252 nm. The three drugs were satisfactorily resolved with Rf values of 0.21, 0.79 and 0.42 mins for Atorvastatin calcium, Fenofibrate and Ezetimibe respectively. The developed method was validated for linearity, accuracy, precision, robustness and specificity studies as per the ICH guidelines. The method was found to be linear over concentration ranges of 200-1200 ng/μl, 50-300 ng/μl and 100-350 ng/μl for Atorvastatin calcium, Fenofibrate and Ezetimibe respectively. Recovery studies indicated accurate recoveries of the three drugs using standard addition method. The % RSD values for the intra-day and inter-day precision studies were found to be 1.25, 1.75 and 1.44 and 1.22, 1.72 and 1.46 for Atorvastatin calcium, Fenofibrate and Ezetimibe respectively. The HPTLC method was successfully applied to the analysis of all the three drugs in a pharmaceutical tablet formulation. No chromatographic interference from the tablet excipients was seen in this method. The acid degraded solutions of Atorvastatin calcium, Fenofibrate and Ezetimibe, when applied along with pure API’s did not showed any interference from peaks of degradation products....
NSAIDs are often used for their anti-inflammatory, analgesic, and/or antipyretic effects; it is well known that NSAIDs have the potential to cause gastrointestinal (GI) bleeding through a variety of mechanisms related to their topical and systemic use. Hence the combination of NSAID with a proton pump inhibitor is beneficial for the patients on long term treatment with NSAIDs. An attempt was done to develop simple precise, accurate and validated reverse phase HPLC method for the simultaneous estimation of omeprazole and ketoprofen in bulk and in synthetic mixture using C18 column (Hypersil, 250mm x 4.5 mm) with acetonitrile: 0.02 M potassium dihydrogen phosphate solution (With pH 4.0 adjusted using 1% orthophosphoric acid) (45: 55 v/v) as a mobile phase, at a flow rate of 1.0 ml/min and detection was done at 279.0 nm. The retention time for omeprazole and ketoprofen was found to be 4.06 and 7.03 min, respectively. Linearity of omeprazole and ketoprofen was found in the range of 4-24 μg/ml and 5-30 μg/ml respectively. The percentage assay of omeprazole and ketoprofen was found between 99% to 101%. The statistical parameters were found within range. The result of assay, recovery studies and its statistical validation data indicate high degree of precision and accuracy of the method....
A simple, accurate, validated and reproducible UV-Spectrophotometric method has been developed for the simultaneous estimation of Amlodipine Besylate and Nebivolol in both bulk and tablet formulation. Amlodipine and Nebivolol in combined tablet formulation were estimated by using the multicomponent mode at 361 nm for Amlodipine and 281 nm for Nebivolol in their solution in methanol: water (90:10). The Beer’s law obeyed the concentration range of 10-170µg/ml for both Amlodipine and Nebivolol. Mean recovery of 99.84% for Amlodipine and 99.64% for Nebivolol respectively signifies the accuracy of the method. The methods were validated by accuracy, precision, robustness, ruggedness, LOD & LOQ for both Amlodipine and Nebivolol. The limit of detection for Amlodipine and Nebivolol were 0.565 and0.198.The limit of quantification for Amlodipine and Nebivolol were 1.71 and 0.60. This method can be used for the routine simultaneous estimation of Amlodipine Besylate and Nebivolol in industries and other analytical laboratories....
Two simple, precise and cost effective spectrophotometric methods have been developed for the estimation of Sertaconazole nitrate in bulk and its pharmaceutical formulations. Method A is based on calculation of Area under Curve (AUC) for analysis of Sertaconazole nitrate in the wavelength range of 252.0 – 268.0 nm. Method B first order derivative spectroscopic method in which the wavelength selected 221nm. In both the Methods drug shows linearity in the concentration range of 10-50 μg/ml. Results of analysis for both the methods were validated statistically and by recovery studies. The proposed methods are found to be free from interference of excipients and are successfully applied to estimation of the amount of Sertaconazole nitrate in bulk and pharmaceutical dosage forms....
A stability indicating, simple, economic, rapid, precise and sensitive reverse phase high performance liquid chromatography method was developed and validated for determination of Atazanavir Sulfate in pharmaceutical dosage form. The quantitative determination of Atazanavir Sulfate was performed on an BDS Hypersil C18, 250 mm X 4.6 mm, 5 µm, stainless steel analytical column from Thermoscientific with mobile phase consist of Acetonitrile: 0.02M potassium dihydrogen ortho phosphate (KH2PO4) (70:30 %v/v), pumped at a constant flow rate of 1 mL min-1. The detection is carried out using variable wavelength UV-Vis detector set at 249.5 nm. The method shows good peak shape, minimal tailing, with retention time 3.77 min for Atazanavir Sulfate. The drug was subjected to acidic, alkaline, oxidation, photo-degradation to apply stress conditions. The developed method was able to separate degradation product generated under forced degradation studies. The developed method was validated as per ICH guidelines for the parameters such as specificity, linearity, accuracy, precision, limit of detection, limit of Quantitation and found to be satisfactorily. The response was linear in the drug concentration range of 10-60 µg mL-1 (r2 = 0.998). The proved to be suitable for stability testing, homogeneity testing and quality control of this compound in pharmaceutical dosage form....
Simple, accurate, sensitive and precise Spectrophotometric and Chemometric methods were developed and validated for determination of Nifuroxazide (Nx) in presence of its alkaline degradation products. Two spectrophotometric methods were investigated, the first one is a second derivative spectrophotometric (2D) determination of Nx in presence of its alkaline degradation products by measuring the peak amplitude at ?=278 nm which corresponds to (zero crossing) of its degradates. While, the second one is a second derivative ratio spectra ( 2DD) which could successfully determine without any interference from its degradates at ?=290.8, The percentage recoveries of pure was found to be 99.97�±1.505 & 99.83�±1.401 for (2D) & ( 2DD) respectively. Chemometric-assisted spectrophotometric methods were also applied as classical least squares (CLS), principal component regression (PCR) and partial least squares (PLS), the percentage recoveries for Nx were 99.49 �±2.60 , 98.914 �±1.68 and 99.08 �±1.38 for CLS, PCR and PLS, respectively. The developed chemometric models have the advantage that they are not only determine the drug in presence of its degradates but also quantify the degradates in the mixtures. All the developed methods were successfully applied for the determination of Nx in its bulk powder and dosage form and the validity of the proposed methods was further assessed by applying the standard addition technique. The developed methods were statistically compared with each other and with a reported method and no significant difference were observed regarding both accuracy and precision, all the developed methods have been validated according to ICH guidelines....
A sensitive and reproducible method is described for the quantitative determination of telmisartan in the presence of its degradation products. Separation was carried out on Merck HPTLC aluminium sheets of silica gel 60 F254 using ethyl acetate: benzene: methanol (9.0: 6.5: 3.5, v/v/v) as mobile phase. This system was found to give compact spots for telmisartan after double development (Rf value of 0.51 ? 0.02). The second order polynomial regression analysis data was used for the regression line in the range of 500-6000 ng/spot. The method has been successively applied to pharmaceutical formulation. No chromatographic interference from the tablet excipients was found. Method was validated in terms of precision, robustness, recovery and limits of detection and quantitation. Drug was subjected to acid and alkali hydrolysis, oxidation, dry heat, wet heat treatment and photo degradation. Significant degradation was observed in all stress conditions. An attempt was made to separate the acid degradation product using preparative TLC and was further identified by LC-MS. The developed method could effectively separate the drug from its degradation products, so it can be employed as stability indicating method for routine quality control of telmisartan....
A simple, precise, accurate and stability indicating UV-method have been developed and validated for estimation of Olmesartan. Many experiments were conducted by taking combination of drugs & also by single drug but no suitable validation with stability study was reported. Olmesartan has the absorbance maxima at 257nm.Method A involves method development and validation, showed sharp peak at 257nm.Method B involves forced degradation study. All the methods utilize methanol as solvent. Linearity for the detector response was observed in the concentration range of 5-35µg/ml. Validation experiments were performed to demonstrate System suitability, Specificity, Precision, Linearity, Accuracy Precision, robustness, ruggedness, LOD, &LOQ. Furthermore stability studies of Olmesartan were carried out under acidic, alkali, neutral, oxidation &photolytic degradation as per stability indicating assay methods. The results of analysis have been validated and recovery studies were carried out by adding specific drug amount (80%, 100%, 120%) and shows recovery studies in the range (99.45 -100.38) %. The proposed method can be successfully applied for method development, validation and stability study of Olmesartan....
A simple, rapid and sensitive extractive spectrophotometric method has been developed for the assay of sildenafil citrate (SILC) in pure and pharmaceutical formulations (Virecta tablets). This method is based on the formation of chloroform soluble ion-pair of SILC with bromothymol blue (BTB) and methylene chloride soluble ionpair of SILC with bromophenol blue (BPB) and eriochrome blue black R (EBBR) in borax buffer of pH 3 and volume 1mL for BTB while acetate buffer of pH 3 and volume 1mL for BPB and universal buffer of pH 2 and volume 1.5 mL for EBBR with absorption maximum at 415, 420 nm and 510 nm for BTB, BPB and EBBR reagents, respectively. Reaction conditions were optimized to obtain the maximum colour intensity. The absorbance was found to increase linearly with the increase in SILC concentration, which was corroborated by the calculated correlation coefficient values (0.9909, 0.9901 and 0.9917 for BTB, BPB and EBBR reagents, respectively). The systems obeyed Beerâ��s law over the concentration range of 1-40, 1-50 and 3-70 �µg mL-1 for BTB, BPB and EBBR, respectively. Various analytical parameters have been evaluated and the results have been validated by statistical data. No interference was observed from common excipients present in pharmaceutical formulations....
A rapid, economic, sensitive and reproducible colorimetric method for quantitative estimation of Amikacin from bulk and pharmaceutical formulations has been developed. The method employs 1% cobalt nitrate reagent in presence of 2Molar sodium hydroxide to form violet color complex with Amikacin. The concentration of Amikacin over a range of 1.6-4.8 miligram/mililiter was found to obey Beer-lambert’s law. The developed method was validated in accordance with ICH Q2 guidelines. The mean percentage recovery was found to be 99.88% to 100.09%. The developed method was compared with reported RP-HPLC method. The developed method could be used for routine analysis of Amikacin in bulk and formulation due to simplicity, ease of operation and short time required for quantification....
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