Jagdish Parasrampuria

Quantitation of Ciprofloxacin Hydrochloride and Norfloxacin in Tablets Using High-Performance Liquid Chromatography

AbstractA stability-indicating high-performance liquid chromatography method for the quantitation of ciprofloxacin and norfloxacin in tablets (the only dosage form available at present) has been developed. The method is precise and accurate with a percent relative standard deviation based on 5 readings of 1.2 and 1.4 for ciprofloxacin and norfloxacin, respectively. A number of inactive ingredients present in the tablets did not interfere with the assay procedures. The addition of hydrochloric acid in the extraction procedure was necessary for the quantitative recovery and reproducible results. The recovery from the synthetic mixtures was quantitative. Both the drugs (quinolones) appear to be very stable since 10 minute boiling with either sulfuric acid or sodium hydroxide solution caused very little decomposition.

CHEMICAL STABILITIES OF FAMOTIDINE AND RANITIDINE HYDROCHLORIDE IN INTRAVENOUS ADMIXTURES

The chemical stabilities of famotidine and ranitidine hydrochloride solutions in 5% dextrose and 0·9% sodium chloride injections have been studied using high‐performance liquid chromatographic methods (HPLC). Both the drugs were stable for at least 15 days (loss in potency of less than 10%) at 25°C and 63 days at 5°C. Both drugs were comparatively less stable in 5% dextrose injection than in 0·9% sodium chloride injection. The loss in the potency of phenol, which is added as a preservative to ranitidine hydrochloride injection, was significant in both the vehicles. However, the addition of preservative in a single dose vial is not considered necessary.

Quantitation of Phenylephrine Hydrochloride in Pharmaceutical Dosage Forms

AbstractA reverse phase high-pressure liquid chromatography method for the quantitation of phenylephrine hydrochloride in a variety of pharmaceutical dosage forms has been developed. The developed method did not require the use of a counter-ion t o increase the retention time of phenylephrine. The method is simple, accurate, precise and reproducible with a percent relative standard deviation of 0.54 based on 6 injections. The results were in excellent agreement with the results obtained using a colorimetric method. The separation between phenylephrine, the internal standard and other ingredients is greatly affected by pH changes (between 5.9-6.1) and the particle size of the column materials (5 micron versus 10 micron). A number of other active ingradinents brompheniramine maleate, chlopheniramine maleate, phenylpropanolamine and guaifenesin, etc. and the excipients such as parabens and sodium benzoate did not interfere with the assay procedure.

Moist-Heat Sterilization and the Chemical Stability of Heat-Labile Parenteral Solutions

The impact of moist-heat sterilization (autoclaving) on the chemical stability of parenteral solutions was examined using two heat-labile products, clindamycin phosphate and succinylcholine chloride injections, as examples. A nonisothermal kinetic model was used to predict the extent of product degradation during autoclaving. The predicted results were found to be in close agreement with the experimental data. For the same peak temperature, a greater loss of product was shown by using a cycle with a higher F0. On the other hand, a higher peak-temperature cycle resulted in less product degradation for the same F0 value. The benefit of a high-temperature cycle was further illustrated by the fact that less chemical degradation for both products was produced by a 122 degrees C cycle with an F0 of 11 as compared to that which occurred during a 116.5 degrees C cycle with an F0 of 8. Although clindamycin phosphate was found to be highly unstable during a conventional autoclaving process, predicted data indicate that a UHT (Ultra-High Temperature) process may be used to sterilize this product with acceptable degradation.

Quantitation of Sulfacetamide, Sulfadiazine, Sulfamerazine and Sulfame Thazine in Various Cominations Dsing High-Performance Liquid Chromatography

AbstractA reverse phase high-performance liquid chromatography method for the quantitation of sulfacetamide, sulfadiazine, sulfamerazine, and sulfamethazine in various combinations has been developed. The method is simple, accurate, precise and reproducible. The percent relative standard deviations based on 6 injections were 2.1, 0.6, 1.9, and 1.6 for sulfacetamide, sulfadiazine, sulfamerazine, and sulfamethazine, respectively. The ratio of peak heights (drug/internal standard) wer closely related (r value 0.99 or better) to concentrations (± 20% of the standard solution concentrations). The results of synthetic mixtures showed quantitative recovery and method was successfully applied to commercial dosage forms (tablets and suspension). Extraction of sulfa drugs from the dosage forms required a very simple procedure.

A Study of The Moisture-Uptake Kinetics of a Hygroscopic Pharmaceutical Powder

AbstractThe moisture-uptake kinetics of a hygroscopic powder, sodium heparin contained in a cylindrical container, was determined using a novel moisture-uptake measuring device under a constant convective air flow. The amount of moisture uptake increased with the increase in the relative humidity of the air. The effect of powder-bed height on the total amount of moisture uptake was found to be significant only at the highest relative humidity (75%) evaluated in this study. However, the percent of weight increase of the powder as a result of moisture uptake decreases as the height of the powder bed increases. The results of this study are explained by the dynamic nature of the moisture-uptake process associated with the instrument.

Important Information for Readers of High-Performance Liquid Chromatography Literature

AbstractImportant information for developing an internal standard for high-performance liquid chromatography has been presented in a tabular form. If acetonitrile is substituted for methanol, the column lives are longer and costly repairs of the chromatograph are not needed that often. Approximately 1% of acetonitrile can be substituted for 2% of methanol.

Colorimetric Determination of Piroxicam in Capsules

AbstractA 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.

CHEMICAL STABILITIES OF ISOETHARINE HYDROCHLORIDE, METAPROTERENOL SULPHATE AND TERBUTALINE SULPHATE AFTER MIXING WITH NORMAL SALINE FOR RESPIRATORY THERAPY

The chemical stabilities of isoetharine hydrochloride inhalation solution, metaproterenol sulphate inhalation solution and terbutaline sulphate injection, after diluting 1 in 10 with sodium chloride 0·9% injection were studied. On storing the solutions in amber‐coloured syringes, they were stable for at least 120 days at 5°C. At 25°C they were also stable for 120 days except that isoetharine solution discoloured and lost 7·8% of its potency after 90 days of storage. There was a new peak in the chromatogram from the decomposition product. All other solutions remained clear for 120 days at both temperatures. The initial and final pH values were similar except that after 120 days at 25°C, the pH value of terbutaline solution had increased from 4·9 to 5·4.

Quantitation of 4-(4-Chl0R0Phenyl)-2-Pyrr0Lidin0Ne in Baclofen Powder and Tablets

AbstractA high-pressure liquid chromatography method to quantify 4-(4-chlorophenyl)-2-pyrrolidinone which is present as an impurity in baclofen powder and its dosage forms has been developed. The USP-NF method for the determination of 4-(4-chlorophenyl)-2-pyrrolidinone in powder is based on TLC and is only qualitative. The developed method was successfully used to quantify 4-(4-chlorophenyl)-2-pyrrolidinone in powder (USP-NF limit 1%) and in tablets (USP-NF limit 5%). The method is accurate and reproducible with a percent error of 4% for powder and 3% for tablets.