ABSTRACT
Different analytical tasks in the pharmaceutical analysis can be classified according to the separation problems into three main groups: trace analysis, assay methods and separation of closely related compounds including isomers. The most important requirements of high-performance liquid chromatographic (HPLC) methods with respect of the separation problems are summarized. Considerations and recommendations for the selection of the most applicable HPLC system to solve particular analytical problems are discussed. HPLC methods can be compared on the basis of the system resolution (SR) and system selectivity (SS). Criteria developed for the characterization of HPLC methods considering the difficulties created by the different analytical problems are established. The principles of the selection of the most applicable separation systems are demonstrated through some practical examples in pharmaceutical analysis.
Subject(s)
Pharmaceutical Preparations/analysis , Chromatography, High Pressure Liquid/methods , Ergotamine/analysis , Sulfinpyrazone/analysisSubject(s)
Platelet Aggregation/drug effects , Anti-Inflammatory Agents/analysis , Anti-Inflammatory Agents/pharmacology , Aspirin/pharmacology , Chemical Phenomena , Chemistry , Dipyridamole/analysis , Dipyridamole/pharmacology , Heterocyclic Compounds/analysis , Heterocyclic Compounds/pharmacology , Humans , Imidazoles/analysis , Imidazoles/pharmacology , Phthalazines/analysis , Phthalazines/pharmacology , Pyridazines/analysis , Pyridazines/pharmacology , Pyridines/analysis , Pyridines/pharmacology , Pyrimidines/analysis , Pyrimidines/pharmacology , Quinazolines/analysis , Quinazolines/pharmacology , Quinolines/analysis , Quinolines/pharmacology , Sulfinpyrazone/analysis , Sulfinpyrazone/pharmacologyABSTRACT
An HPLC method for the simultaneous determination of sulfinpyrazone and its p-hydroxy, sulfone, sulfide and p-hydroxysulfide metabolites in human plasma and urine samples was developed. Optimization with regard to sample preparation and chromatographic conditions was investigated. In the final procedure samples were acidified with HCl, extracted with a 1 + 1 (vol/vol) mixture of 1-chlorobutane and chloroform; urine extracts were re-extracted with citrate buffer (pH 4.5). HPLC was performed on reversed phase (RP 8) columns with a 48 + 52 (vol/vol) mixture of ethanol and citrate buffer (pH 2.5) as the mobile phase. The lower limit of detection for sulfinpyrazone and the sulfide metabolite is 10 ng/ml, for the other metabolites it is 50 ng/ml. An example of application of this procedure to pharmacokinetic studies in a volunteer receiving a single oral dose of sulfinpyrazone is given.
Subject(s)
Sulfinpyrazone/analysis , Chromatography, High Pressure Liquid , Drug Stability , Humans , Kinetics , Solvents , Spectrophotometry, Ultraviolet , Sulfinpyrazone/blood , Sulfinpyrazone/urineABSTRACT
A high-performance liquid chromatographic method has been developed for the simultaneous determination of azobenzene and hydrazobenzene in phenylbutazone and sulfinpyrazone raw materials and formulations. The drug raw material or formulation is shaken with 1N NaOH and n-hexane and centrifuged. The n-hexane layer is injected into a chromatograph equipped with a 10-micron cyano-amino bonded phase column. Azobenzene and hydrazobenzene are detected at 313 and 254 nm, respectively; the sensitivities are approximately 1 and 2 ppm, respectively, in the raw materials and formulations.
Subject(s)
Azo Compounds/analysis , Phenylbutazone/analysis , Phenylhydrazines/analysis , Sulfinpyrazone/analysis , Chromatography, High Pressure Liquid/methods , Drug ContaminationABSTRACT
A method for the quantitative determination of sulphinpyrazone in plasma and urine is described. The drug is extracted from the acidified aqueous phase with 1-chlorobutane-ethylene dichloride (4:1) and separated from its metabolites by high-performance liquid chromatography on 5-mum LiChrosorb using dichloromethane-ethanol-water-acetic acid (79.1:19:1.9:0.002) as the mobile phase. The sensitivity limit is 0,2mug/ml using a 1-ml sample. Examples of applications are given.
