Method Transfer Evaluation for Digital Derivative Spectrophotometry Through its Resolution Parameter Comparison of Different Computer Programs.

The application assessment of different programs was performed with equivalence tests for method transfer pro second-order derivative spectrophotometry. The digital second-order derivative spectra were calculated on different instruments; GBC Scientific Equipment Cintra 20 (Cintral v.2.

The evaluation of short- and long-term stability studies for brimonidine in aqueous humor by DPV/BDDE method-possible application for direct assay in native samples.

A novel voltammetric method was developed for brimonidine (BRIM) determination in deproteinized aqueous humor, simplifying preparation of biological samples for analysis for stability studies. The differential pulse voltammetric (DPV) method using boron doped diamond electrode (BDDE), based on characteristic oxidation peaks, was proposed and successfully applied. The linearity range was within 5.

Evaluation of angiotensin-converting enzyme inhibitor's absorption with retention data of micellar thin-layer chromatography and suitable molecular descriptor.

Twelve angiotensin-converting enzyme (ACE) inhibitors were studied to evaluate correlation between their absorption (ABS) data available in the literature (22-96%) and hydrophobicity parameters (km and Pm/w) obtained in micellar thin-layer chromatography (MTLC) using Brij 35. The theoretical considerations showed that the geometric molecular descriptor-volume value (Vol) should be considered as an independent variable simultaneously with calculated hydrophobicity parameters in multiple linear regression analysis to obtain reliable correlation between ACE inhibitor's absorption and lipophilicity (calculated KOWWINlog P) and that captopril should be excluded from further correlations. The results of MTLC confirmed that between the two hydrophobicity parameters km and Pm/w, for absorption prediction of 11 ACE inhibitors, the micelle-water partition coefficient Pm/w provided higher correlation (R(2) = 0.

Inter-laboratory verification of European pharmacopoeia monograph on derivative spectrophotometry method and its application for chitosan hydrochloride.

Inter-laboratory verification of European pharmacopoeia (EP) monograph on derivative spectrophotometry (DS) method and its application for chitosan hydrochloride was carried out on two generation of instruments (earlier GBC Cintra 20 and current technology TS Evolution 300). Instruments operate with different versions of Savitzky-Golay algorithm and modes of generating digital derivative spectra. For resolution power parameter, defined as the amplitude ratio A/B in DS method EP monograph, comparable results were obtained only with algorithm's parameters smoothing points (SP) 7 and the 2nd degree polynomial and those provided corresponding data with other two modes on TS Evolution 300 Medium digital indirect and Medium digital direct.

In vitro modeling of angiotensin-converting enzyme inhibitor's absorption with chromatographic retention data and selected molecular descriptors.

Set of nine angiotensin-converting enzyme inhibitors (enalapril, quinapril, fosinopril, lisinopril, cilazapril, ramipril, benazepril, perindopril and moexipril) were studied to evaluate the correlation between their intestinal absorption and salting-out thin-layer chromatography hydrophobicity parameters (RM(0) or C0) obtained by ascending technique applying four different salts, (NH4)2SO4, NH4NO3, NH4Cl and NaCl as mobile phases. The best correlations between KOWWIN logP and both hydrophobicity parameters, RM(0) and C0, (R(2)>0.850) were observed for NaCl (1.

Correlation between ultra-high performance liquid chromatography-tandem mass spectrometry and reversed-phase thin-layer chromatography hydrophobicity data for evaluation of angiotensin-converting enzyme inhibitors absorption.

In this research seven ACE inhibitors (enalapril, quinapril, fosinopril, lisinopril, cilazapril, ramipril, benazepril) were studied to evaluate the correlation between their absorption and ultra-high performance liquid chromatography-tandem mass spectrometry (UHPLC-MS) and reversed-phase thin-layer chromatography (RP-TLC) hydrophobicity data (φ(0) or C(0) parameters, respectively). Their absorption values were in the range of 25-60%, while calculated KOWWIN logP values were from -0.94 to 6.

Lipophilicity Examination of Some ACE inhibitors andHydrochlorothiazide on Cellulose in RP Thin-Layer Chromatography.

In this assay, the evaluation of lipophilicity of four ACE-inhibitors and hydrochlorothiazide (HCTZ) with RP-TLC on cellulose layers was described using three binary solvent systems. The selected ACE inhibitors had sufficiently different structures which can indicate the method suitability for their lipophilicity evaluation as the model substances in comparison with HCTZ. In addition, the linear relationship between the RM-values and composition of mobile phases was established in the current study.

A PAMPA assay as fast predictive model of passive human skin permeability of new synthesized corticosteroid C-21 esters.

The permeation properties of twenty newly synthesized α-alkoxyalkanoyl and α-aryloxyalkanoyl C-21 esters of standard corticosteroids: Fluocinolone acetonide, dexamethasone, triamcinolone acetonide and hydrocortisone were established using a PAMPA assay (70% silicone oil and 30% isopropyl myristate). The data were compared with parent corticosteroids with addition of mometasone furoate and hydrocortisone acetate. All newly synthesized corticosteroid C-21 esters have effective permeability coefficients higher then -6, mostly followed with high values of retention factors and low permeation.

An application of second-order UV-derivative spectrophotometry for study of solvolysis of a novel fluocinolone acetonide ester.

A novel topical corticosteroid FA-21-PhP, 2-phenoxypropionate ester of fluocinolone acetonide, has been synthesized in order to investigate the possibility of decreasing systemic side effects. In this study model system for in vitro solvolytic reaction of FA-21-PhP has been analyzed in ethanol/water (90:10, v/v) with excess of sodium hydrogen carbonate. The selected conditions have been used as in vitro model for activation of corticosteroid C-21 ester prodrug.

SPE and large-volume sample stacking in MEKC for determination of doxycycline in biological fluids: comparison of direct injection to SPE-MEKC.

A novel and simple method has been developed for the determination of doxycycline (DOX) in biological fluids. The method is based on SPE, large-volume sample stacking (LVSS) and MEKC with UV-DAD detection. Six SPE cartridges have been used in investigation for sample clean up and pre-concentration (Supelco LC-8, LC-18, LC-SCX, and LC-WCX, as well as Strata-X and X-C).

Determination of caffeine and associated compounds in food, beverages, natural products, pharmaceuticals, and cosmetics by micellar electrokinetic capillary chromatography.

A method is described for quantitating caffeine, theobromine, theophylline, paracetamol, propyphenazone, acetylsalicylic acid, salicylic acid, and codeine phosphate in corresponding real samples of food, beverages, natural products, pharmaceuticals, and cosmetic preparations by micellar electrokinetic capillary chromatography. The separation is carried out at 25 degrees C and 25 kV, using a 20 mM phosphate buffer (pH 9.0), 80 mM sodium dodecyl sulfate, and 7.

Optimal conditions for determination of zinc bacitracin, polymyxin B, oxytetracycline and sulfacetamide in animal feed by micellar electrokinetic capillary chromatography.

A separation technique for zinc bacitracin, polymyxin B, oxytetracycline and sulfacetamide in animal feedstuffs by micellar electrokinetic capillary chromatography (MEKC) was developed. The running buffer was 20 mmol l(-1) borate, 20 mmol l(-1) phosphate, pH 8.4, containing 20 mmol l(-1) sodium dodecylsulphate and 10% (v/v) methanol.

Micellar electrokinetic capillary chromatography determination of zinc bacitracin and nystatin in animal feed.

An MEKC procedure was developed for the separation of zinc bacitracin (Zn-BC) and nystatin (NYS) in mixtures and in animal feedstuff. The running buffer was 15 mM borate/19 mM phosphate, pH 8.2, containing 20 mM SDS and 10% v/v methanol.

Development of the second-order derivative UV spectrophotometric method for direct determination of paracetamol in urine intended for biopharmaceutical characterisation of drug products.

Paracetamol is a widely used nonsalicylate analgesic and antipyretic drug. The existing methods for the determination of paracetamol in biological fluids are mainly HPLC techniques, although there are some reported methods based on spectrophotometric determinations. However, all these methods involve some extraction or derivatisation procedures.

Photochemical degradation of solid-state nisoldipine monitored by HPLC.

The photochemical degradation of solid-state nisoldipine, 1,4-dihydropyridine calcium antagonist, was investigated under daylight and UV light conditions. Degradation products were identified by using the retention times of corresponding standards and quantified by high-performance liquid chromatographic method. The daylight illumination induced appearance of nitrosophenylpyridine, while formation of second degradation product, nitrophenylpyridine, was observed only upon UV light illumination.