Stabilized normal-phase high-performance liquid chromatographic analysis of aspirin and salicylic acid in solid pharmaceutical dosage forms.

A simultaneous analysis of aspirin and nonaspirin salicylates in solid pharmaceutical dosage forms is described. Two separate extraction procedures are employed, one for plain aspirin tablets and one for tablets containing aspirin plus buffers or antacids. The analyses of the extracted samples are accomplished by a stabilized normal-phase high-performance liquid chromatographic (HPLC) procedure. Prepared samples and standards are stable for up to 24 h, and the methodology is suitable for an automated HPLC system.

Evaluation of antacid suspensions containing aluminum hydroxide and magnesium hydroxide.

Liquid antacid suspensions containing aluminum hydroxide and magnesium hydroxide were evaluated for composition, antacid properties, and product quality. The equivalent aluminum oxide and magnesium hydroxide content was determined by chelatometric titration, and sodium content was determined by flame photometry. Antacid properties measured were acid-consuming capacity, antacid effectiveness (preliminary antacid test, acid-neutralizing capacity test), and pH-stat titration. Content uniformity, consistency of the antacid properties, and microbiological content were examined for each product. Data are presented for 36 products for which samples from four or more lots were obtained. The ratio of percentage of equivalent aluminum oxide to percentage of magnesium hydroxide ranged from 1:0.6 to 1:3.5; this range allows for selection of the desired balance between the laxative effect of magnesium hydroxide and the constipating effect of aluminum hydroxide. Based on a daily dose of 280 meq of antacid, the sodium content of the products tested ranged from less than 2% to approximately 45% of the 500 mg per day of sodium allowed in a sodium-restricted diet. The concept of bioavailability was related to the amount of the antacid reacting at pH 3, 37 degrees C during the estimated gastric residence time of 15 minutes. Antacid suspensions are available which will react almost completely (neutralizing greater than 90% of the theoretical quantity of acid) during the estimated gastric residence time. Approximately 4% of the samples contained unacceptable numbers of bacteria. An antacid suspension cannot be adequately evaluated by a single test; choice of a product should be based on an evaluation that integrates several characteristics including sodium content, time and volume required to neutralize a given amount of acid, and uniformity of content.

Novel method of derivatization of an amidinourea (lidamidine) for GLC analysis.

A new quantitative GLC method for analysis of lidamidine hydrochloride (I) was developed. The method was based on derivatization of I to 1-(2,6-dimethylphenyl)-4-methylamino-dihydro-1,3,5-triazin-2-one (II) using dimethylformamide dimethylacetal reagent. Compound II was synthesized and characterized by IR, NMR, mass spectrometry, and elemental analysis. The assigned structure was in agreement with characterization analyses. Cyclization of I to a triazinone using dimethylformamide dimethylacetal reagent presented a new route for the preparation of II.