Quantitation of Cefaclor in Pharmaceutical Dosage Forms Using High Performance Liquid Chromatography

A stability-indicating high-performance liquid chromatography for the quantitation of cefaclor in pharmaceutical dosage forms has been developed. The method is accurate and precise with a percent relative standard deviation of 1.2 based on 5 readings. A number of inactive ingredients present in the capsules and suspensions did not interfere with the assay procedure. The extraction procedure from the dosage forms is very simple. The recovery from the synthetic mixtures was quantitative. The capsules which had expired 3 years ago lost only 3% of the potency. The drug appears to be very sensitive to strong acids or bases since a 5 minute boiling caused 100% degradation of drug in both the solutions.     

Quantitation of Cefaclor in Pharmaceutical Dosage Forms Using High Performance Liquid Chromatography

Abstract

A stability-indicating high-performance liquid chromatography for the quantitation of cefaclor in pharmaceutical dosage forms has been developed. The method is accurate and precise with a percent relative standard deviation of 1.2 based on 5 readings. A number of inactive ingredients present in the capsules and suspensions did not interfere with the assay procedure. The extraction procedure from the dosage forms is very simple. The recovery from the synthetic mixtures was quantitative. The capsules which had expired 3 years ago lost only 3% of the potency. The drug appears to be very sensitive to strong acids or bases since a 5 minute boiling caused 100% degradation of drug in both the solutions.     

Stability of Omeprazole Solutions at Various ph Values as Determined by High-Performance Liquid Chromatography

A stability-indicating HPLC assay method for the quantitation of omeprazole has been developed. The developed method was used to study the effect of pH on the stability of omeprazole and to quantify the drug in capsules. The excipients present in the capsules did not interfere with the assay procedure. The pH-rate profile curve indicated that the maximum stability was at pH 11. Below pH 7.8, the decomposition was very fast. The decomposition constants have a direct relationship with the H+ concentrations of the solutions.     

Stability of Omeprazole Solutions at Various ph Values as Determined by High-Performance Liquid Chromatography

Abstract

A stability-indicating HPLC assay method for the quantitation of omeprazole has been developed. The developed method was used to study the effect of pH on the stability of omeprazole and to quantify the drug in capsules. The excipients present in the capsules did not interfere with the assay procedure. The pH-rate profile curve indicated that the maximum stability was at pH 11. Below pH 7.8, the decomposition was very fast. The decomposition constants have a direct relationship with the H+ concentrations of the solutions.     

Quantitation of fluoxetine hydrochloride in capsules using high-performance liquid chromatography

A stability-indicating high-performance liquid chromatographic method for the quantitation of fluoxetine hydrochloride in capsules (the only dosage form available) has been developed. The method is accurate and precise with a percent relative standard deviation of 1.04 based on 6 readings. An excellent separation of fluoxetine from methyltestosterone (the internal standard) was achieved, and sharp peaks were obtained by adding acetic acid to the mobile phase. The inactive ingredients present in the capsule powder did not interfere with the assay procedure. The recovery of fluoxetine from the synthetic mixtures was quantitative. The drug appears to be very stable in the acidic medium and highly susceptible to degradation in the basic medium.     

Quantitation of Flurbiprofen in Tablets Using High Performance Liquid Chromatography

A stability-indicating high-performance liquid chromatography method for the quantitation of flurbiprofen in tablets was developed. The method is accurate and precise with a percent relative standard deviation of 0.7 based on 8 readings. A number of inactive ingredients present in the tablets did not interfere with the assay procedure. The extraction procedure from the tablets is very simple. The recovery from the synthetic mixtures was quantitative. The drug appears to be very sensitive to strong acids and bases since a 5 minute boiling caused the degradation of drug (100 %) in both the solutions     

Quantitation of Cephalexin in Pharmaceutical Dosage Forms Using High-Performance Liquid Chromatography

A high-performance liquid chromatography method has been developed to quantify cephalexin in pharmaceutical dosage forms, capsules, pediatric drops and suspensions. The method is accurate and precise with a percent relative standard deviation of 0.8 based on 6 readings. There is no interference from a variety of excipients present in the dosage forms. The procedure for the extraction of cephalexin from the dosage forms is very simple. The method is stability indicating since a sample decomposed using sodium hydroxide showed very little potency and new peaks in the chromatogram. In the powder form cephalexin appears to be very stable.     

Colorimetric Determination of Piroxicam in Capsules

A simple colorimetric procedure to quantify piroxicam in capsules has been developed. The method is based on the reaction between piroxicam and 4-aminoantipyrine producing an orange color which can be measured at 490 nm. The method is accurate and precise with a percent relative standard deviation of 0.8 based on 5 readings. The results compared very well with the results obtained using the HPLC procedure. The extraction of piroxicam from the capsule powder is very simple which requires only 4 minutes, versus a 30 minute mechanical shaking recommended by the USP-NF. The results of the decomposed samples were similar to the results obtained using the HPLC method.     

Quantitation of Cephalexin in Pharmaceutical Dosage Forms Using High-Performance Liquid Chromatography

Abstract

A high-performance liquid chromatography method has been developed to quantify cephalexin in pharmaceutical dosage forms, capsules, pediatric drops and suspensions. The method is accurate and precise with a percent relative standard deviation of 0.8 based on 6 readings. There is no interference from a variety of excipients present in the dosage forms. The procedure for the extraction of cephalexin from the dosage forms is very simple. The method is stability indicating since a sample decomposed using sodium hydroxide showed very little potency and new peaks in the chromatogram. In the powder form cephalexin appears to be very stable.     

Quantitation of 5-Flucytosine in capsules using high-pressure liquid chromatography

A stability-indicating reversed phase HPLC method for the quantitation of 5-flucytosine in capsules (the only dosage form available) has been developed. The method requires the use of a mobile phase without any counterion and the samples can be assayed at room temperature. The method is simple, reproducible, precise and accurate with percent relative standard deviation of 0.77 based on 6 readings. There was no interference from the excipients present in capsules and from fluorouracil (the major product of decomposition of 5-flucytosine). The recovery of 5-flucytosine from the synthetic mixtures was quantitative. A simple extraction procedure for 5-flucytosine from the capsules has been developed.     

Stability-Indicating HPLC Method for Betaxolol HCl and Its Pharmaceutical Dosage Forms

Abstract

The present work describes a specific, stability-indicating high-performance liquid chromatographic method for determination of betaxolol HCl and its pharmaceutical dosage forms. Betaxolol HCl was chromatographed on a microbondapak C18 column utilizing a simple mixture of methanol: acetonitrile:0.1% diethylamine (pH 3.0 adjusted using orthophosphoric acid). It was detected at 222 nm. The method is accurate and precise with a percent relative standard deviation of 0.11 based on 6 readings. A number of inactive ingredients present in the dosage forms (eye drop, tablet, gel) did not interfere in the assay procedure. The recovery from synthetic mixtures was quantitative. The extraction procedure from the dosage forms is very simple. The drug appears to be very sensitive to acids (such as sulfuric acid) since 100% of the drug decomposed on boiling for 5 min.     

Quantitation of Acetaminophen, Chlorpheniramine Maleate, Phenyl Toloxamine Citrate and Pseudoephedrine Hydrochloride in Combination in Capsules and Tablets Using High-Performance Liquid Chromatography

A high-performance liquid chromatography method has been developed for the quantitation of acetaminophen, chlorpneniramine and pseudoephedrine in combination in capsules and tablets using a non-polar (μ/C18) column and 3 different mobile phases. A very simple preliminary extraction procedure is required before injecting onto the chromatograph. The method is accurate and precise with percent relative standard deviations based on 6 injections of 0.9, 1.9 and 1.1 for acetaminophen, chlorpneniramine and pseudoephedrine, respectively. Phenyltoloxamine citrate which is often mixed with acetaminophen has also been quantified using the developed method. The percent relative standard deviation based on 6 injections of phenyltoloxamine has been determined to be 1.0.     

Quantitative determination of bucindolol concentration in intact gel capsules using Raman spectroscopy

The ideal quality control method for pharmaceutical products should be capable of rapid nondestructive testing of intact tablets or capsules. Raman spectroscopy using near-infrared excitation is shown to be capable of obtaining useful spectral data directly from drug formulations in gel capsules and from the gel capsules inside blister packs. The Raman data collected from the capsules inside blister packs containing 0-100 mg of the active ingredient (bucindolol), when coupled with multivariate calibration, resulted in a calibration SEP of 3.36 mg. The largest source of error was found to be due to sample inhomogeneity. Even so, the method is shown to have significant potential as a rapid nondestructive quality control method for pharmaceutical samples.     

Effects of coating layer and release medium on release profile from coated capsules with Eudragit FS 30D: an in vitro and in vivo study

The aim of the present research was to evaluate the impact of coating layers on release profile from enteric coated dosage forms. Capsules were coated with Eudragit FS 30D using dipping method. The drug profile was evaluated in both phosphate buffer and Hank’s solutions. Utilization X-ray imaging, gastrointestinal transmission of enteric coated capsules was traced in rats. According to the results, no release of the drug was found at pH 1.2, and the extent of release drug in pH 6.8 medium was decreased by adding the coating layers. The results indicated single-layer coated capsules in phosphate buffer were significantly higher than that in Hank’s solution. However, no significant difference was observed from capsules with three coating layers in two different dissolution media. X-ray imaging showed that enteric coated capsules were intact in the stomach and in the small intestine, while disintegrated in the colon.     

Nuclear Magnetic Resonance Analysis of Phenytoin and Sodium Phenytoin in Solid Dosage Forms

A rapid and specific nuclear magnetic resonance (NMR) spectroscopic method was developed for determining phenytoin and its sodium salt in capsules and tablets. Acetamide was used as the internal standard and 0.5% sodium deuteroxide in deuterium oxide served as the NMR solvent. The concentration of drug per unit dose was calculated from the integration values for the resonance signals of phenytoin at about 7.40 ppm and of the internal standard at about 1.97 ppm. The average recovery value of phenytoin added to synthetic samples, in concentrations ranging from 84 to 122 mg, was 99.9 ± 0.2% (SD) with a coefficient of variation of 0.2%. The method using commercial products gave results comparable to those obtained by the titrimetric and gravimetric methods of USP XX. Excipients of tablets and capsules such as sucrose and lactose did not interfere with the determinations. The proposed method was found suitable for measuring the content uniformity of capsules and tablets, and offered a positive means of identification on phenytoin in these dosage forms.     

Estimation of bottle filling counts for conventional pharmaceutical tablets and capsules

A method has been developed using commonly available data for estimating the number of tablets or hard shell capsules that can be filled into bottles. The single unit volumes of conventional pharmaceutical biconvex tablets and capsules can be calculated from simple geometric relationships, which then can be used to determine the packing fraction of the units in bottles. The packing fractions of capsules and tablets studied in this work ranged from 0.53 to 0.63 and 0.56 to 0.62, respectively, and were dependent on bottle size and shape. This method can be used to assess a variety of packaging configurations computationally during drug product development.     

Quantitation of Cefadroxil in Pharmaceutical Dosage Forms Using High-Performance Liquid Chromatography

A high-performance liquid chromatography method for the quantitation of cefadroxil has been developed. The method has been applied to quantify cefadroxil in pharmaceutical dosage forms (capsules, suspensions and tablets) of 2 different manufacturers. A simple extraction procedure to extract cefadroxil from the dosage forms has been developed. The results were excellent with percent relative standard deviation of 1.2 based on 5 readings. A variety of inactive ingredients present in the dosage forms did not interfere with the assay procedure. After formulating, the suspensions were stable for longer periods at 5^o than recommended on the label.     

Nano-engineered microcapsules of tannic acid and chitosan for protein encapsulation

Tannic acid (TA), a high molecular weight polyphenol of natural origin, was assembled in alternation with chitosan (CH) using a layer-by-layer technique. The deposition of tannic acid and chitosan layers on flat supports was monitored by quartz crystal microbalance, UV-vis spectroscopy, and electrophoretic mobility measurements on microparticles. Hollow (TA/CH)4 capsules were built and their permeability as a function of pH and molecular weight of a penetrating compound was investigated. The pH-permeability threshold for TA/CH capsules is shifted to lower pH for 2 pH units, as compared with commonly used polyallylamine/polystyrene sulfonate capsules. A more pronounced dependence of the TA/CH capsules' permeability on molecular weight of encapsulated substances allows better control over their release properties. Bovine serum albumin was loaded into (TA/CH)4 capsules using a pH-driven method and released by decreasing pH. Biocompatible tannic acid/chitosan films and capsules have advantages toward capsules made of synthetic polyelectrolytes for drug encapsulation and as delivery and depot systems. Incorporating a layer of tannic acid with proved antioxidant and antimicrobial properties into capsule walls, provides defense for encapsulated materials.     

The Use of Radio-Labeled Drug in Early Dosage form Development to Provide a Relation Between Physical Dosage form Characteristics and Bioavailability

A chemical compound in early drug development was used in its radio-labeled form to provide a relation to the physical dosage form characteristics and bioavailability. The ¹⁴C-labeled compound, a dibenzthiepin acetic acid derivative, was recrystallized in the same manner as the cold compound. A procedure was developed such that the crystal type and size obtained was similar to that of the cold compound. The photomicrographs and specific surface area of both cold and ¹⁴C-1abeled material were equivalent. Capsules, prepared with both cold and ¹⁴C-labeled material, were demonstrated to have equivalent in vitro dissolution profiles.

The capsules containing the ¹⁴C-labeled material were found to be well absorbed when administered to cynomolgus monkeys. Assuming the monkey is a good absorption model for man, this study provided a preliminary assessment of the bioavailability of the compound in man. It also established preliminary control parameters for the raw material and the dissolution of the capsules. These controls would then be used for monitoring capsules intended for early clinical studies.     

Studies of Hie Effect of Powder Moisture Content on Drug Release from Hard Gelatin Capsules

The in vitro dissolution of model formulations from hard gelatin capsules containing drug: diluent powder mixtures at different moisture levels has been studied. The capsules were filled to a constant porosity of 50%. to contain either sodium barbitone or barbitone in 50:50 mixture with lactose or maize starch, the latter at one of three moisture levels. In addition, capsules containing drug alone were examined. The wettability and polarity indeces of the individual powders and binary mixtures, as well as the permeability and liquid penetration rates of powder beds were also determined.

The presence of either excipient was found to modify the time for 50% drug dissolution (t₅₀) compared with drug alone for all formulations examined, apart from the sodium barbitone: lactose capsules. The rate of drug dissolution was also dependent on the initial powder moisture content for the drug:starch formulations. Open storage of capsules at 20^%/75%. R.lt. generally increased t₅₀figures.

The findings are discussed in terms of the nature of the surfaces of the powder particles, moisture sorption phenomena and factors such as powder bed permeability and water penetitration lates.