Effect of cyclodextrins on the stability of adriamycin, adriamycinol, adriamycinone and daunomycin.

The stability of adriamycin (ADR), adriamycinol, adriamycinone (ADR-ONE) and daunomycin in the presence of alpha-, beta- and gamma-cyclodextrins (CDs) was studied using high-performance liquid chromatography. It was found that alpha-CD did not affect the degradation of tested compounds, beta-CD caused a little effect and gamma-CD resulted in pronounced stabilizing effect. The formation of complexes between ADR and ADR-ONE with CDs was monitored by fluorescence spectroscopy. The fluorescence spectrum of ADR-gamma-CD complex had an activation maximum at 460 nm, emission maximum at 555 nm and a shoulder at 585 nm. A similar finding was observed in case of alpha-CD. In case of beta-CD, the fluorescence intensity at 580 nm peak enhanced less than in case of gamma-CD. With ADR-ONE, alpha-CD did not cause any significant change compared with the spectrum of free molecule. On the other hand, it was noticed that, the fluorescence spectra of ADR-ONE with both beta- and gamma-CD were the same but showed a significant difference to the spectrum of free molecule, especially the molar fluorescence of the 585 nm emission peak.

Determination of barnidipine in human serum and dog plasma by HPLC with electrochemical detection.

Barnidipine is a 1,4-dihydropyridine calcium antagonist. HPLC was conducted on a polybutadiene coated alumina column using an alkaline mobile phase and an electrochemical detector to determine the content of this drug in serum and plasma. A good linear relationship between barnidipine concentration and peak height was found in 5-500 ng/ml with a correlation coefficient of 0.998. The detection limit was 1 ng/ml. The within-day and day-to-day variations were examined for control human serum. Relative standard deviation of within-day assay for serum spiked with 10 ng/ml barnidipine.HCl was 6.9% and the recovery was 104%. A pharmacokinetic study was made in which the time course of barnidipine in dog plasma was followed.

Simultaneous determination of free and bound adriamycin, adriamycinol, adriamycinone and duanorubicin in plasma using column-switching technique and protein-coated pre-columns.

Adriamycin, adriamycinol, adriamycinone and duanorubicin were simultaneously determined by the development of an on-line plasma clean-up system. A short protein-coated Lichrosorb, RP-8, RP-2, CN and muBondapak phenyl as well as ODS silica have been examined for their performance as pre-columns. The drugs and metabolites were separated from weakly retained plasma components through two steps; phosphate buffer saline, pH 7.4 and 15% acetonitrile in 0.1 M sodium dihydrogen phosphate, pH 3. The chromatographic conditions were: ODS/TM column, flow rate 1 ml/min, 35% acctonitrile in 0.1 M sodium dihydrogen phosphate (pH 3) containing 0.3% heptafluorobutyric acid as mobile phase. The detection was carried out using fluorescence monitor operated at an emission 555 nm and excitation 460 nm. Good resolution was obtained within 13 min. This method is reproducible for analysis of drugs and metabolites (99.3-100.1%, CV < 2%) in plasma.

HPLC Determination of some antibilharzial antimonials by extraction of antimony.

The antimonial drug (antimony potassium tartrate, antimony piperazine tartrate or antimony lithium thiomaleate) in aqueous solution or biological fluid is treated with sodium diethyldithiocarbamate in the presence of a suitable masking reagent, the pH is adjusted to 9 +/- 0.5. and the antimony complex extracted with n-hexane and determined by reversed-phase HPLC with an ODS column and detection at 254 nm. The limits of detection are 20 ng (for antimony potassium tartrate and antimony lithium thiomaleate) and 16 ng (for antimony piperazine tartrate).

HPLC determination of niridazole.

A high-performance liquid chromatographic method has been developed for the determination of niridazole in bulk form and in pharmaceutical dosage form. A reversed-phase system, based on an octadecylsilane-bonded stationary phase and a 60:40 v/v methanol/water mobile phase, is used. The detector response at 370 nm is linearly related to the amount injected, over a wide range. The method is sensitive, simple, rapid and precise.

Tetrazolium salts in pharmaceutical analysis II: direct assay of diethylstilbestrol and diethylstilbestrol dipropionate.

A convenient spectrophotometric determination of diethylstilbestrol and diethylstilbestrol dipropionate was developed involving their interaction with triphenyltetrazolium chloride at 50 degrees for 45 min and subsequent measurement of the formazan formed. The significance of extended conjugation within t,e 4,4'-stilbenediol molecule to induce the color reaction is documented. Ideal adherence of color absorption to Beer's law permitted accurate and precise determination of diethylstilbestrol and diethylstilbestrol dipropionate pure forms over the range of 2-22 microgram of diethylstilbestrol/ml. Application of the tetrazolium color reaction to the analysis of diethylstilbestrol dipropionate dosage forms was achieved without prior hydrolysis or extraction.

Colorimetric determination of catecholamines by 2,3,5-triphenyltetrazolium chloride.

A convenient spectrophotometric method was developed for the determination of epinephrine, levarterenol, isoproterenol, and methyldopa by reduction of 2,3,5-triphenyltetrazolium chloride and subsequent measurement of the formazan at 485 nm. With absolute alcohol as the solvent, maximum color absorption was attained in 30 min at 25 degrees in the presence of 0.1 N KOH. Evidence is provided to account for the reduction of the tetrazolium salt at the expense of the epinephrine catechol moiety. In addition to the considerably high values of the molar absorptivities of the chromogen formed, ideal adherence of the color absorption to the Beer-Lambert law permitted a sensitive microdetermination of these catecholamines in both pure forms and pharmaceutical formulations. The tetrazolium interaction was selective. No interference was encountered from common catecholamine antioxidants, adjuvants, or noncatechol degradation products.

Polarographic study of new antibacterial isoxazolium salts: 2,3-dialkyl-5-arylisoxazolium perchlorates.

The polarographic reduction of new antibacterial 2,3-dialkyl-5-arylisoxazolium salts is described. The electrode process involves an irreversible two-electron transfer and is pH independent within the 6.0-10.0 range. In more acidic media, hydrogen waves are observed; at higher pH values, a chemical degradation of the isoxazolium salt proceeds. Values of the half-wave potential of the salts are dependent on the polar contribution of the 5-aryl substituents in terms of the Hammett equation. The in vitro minimum inhibitory concentrations of these compounds are best correlated with Hansch PI values.