Determination of tromethamine in an eye-care pharmaceutical by capillary electrophoresis

Tromethamine [tris(hydroxymethyl)aminomethane] is used as an emulsifying agent, alkaliser and buffering agent in pharmaceutical preparations such as eye-care solutions. A new method for the determination of this compound in an eye-care preparation was developed using capillary zone electrophoresis with indirect UV detection. The method displayed linearity between 2.5 and 25 mg l-1 with a correlation coefficient of 0.9992. The limit of detection was 2.5 mg l-1. Precision and accuracy were determined as relative standard deviation and % deviation, and were found to be 0.42% and 1.62%, respectively. Recovery studies of tromethamine in the pharmaceutical preparation gave a 102.98% recovery.     

Current developments and future trends in solid-phase microextraction techniques for pharmaceutical and biomedical analyses

Sample preparation is important for the isolation and concentration of desired trace components from complex matrices. Sample preparation is the most labor-intensive and error-prone process in analytical methodology, and greatly influences the reliable and accurate determination of analytes. The integration of sample preparation with various analytical instruments is most conveniently achieved by using microextraction techniques and/or microdevices. Solid-phase microextraction (SPME) is both simple and effective, enabling miniaturization, automation and high-throughput performance. Moreover, SPME has reduced analysis times, as well as the costs of solvents and disposal. This review describes current developments and future trends in novel SPME techniques, including fiber SPME, in-tube SPME and related new microextraction techniques. Especially innovative SPME approaches, including multi-well high-throughput sampling, ligand-receptor binding study for pharmacokinetics, direct in vivo sampling, chip-based microfluidic system, and new sampling techniques using intelligent carbon nanotube and temperature-response polymer in pharmaceutical and biomedical analysis are focused items.     

Chromatographic analysis of Passifit multicomponent pharmaceutical syrup

Procedures are developed for the qualitative analysis of a new pharmaceutical preparation, Passifit syrup. The conditions for the separation of the active substances were optimized. Valerian and hop extracts were detected by thin-layer chromatography on Kieselgel 60/Kieselguhr F₂₅₄ plates. Menthol (the volatile component of peppermint oil), thymol and its isomer carvacrol (the components of thyme extract), and sorbic acid (preserving agent) were identified by gas-liquid chromatography on a capillary column with an OV-101 stationary phase and a flame-ionization detector. Luteolin, thymol, rutin, and sorbic acid were identified by reversed-phase HPLC on a Zorbax SB C18 column in a gradient elution mode with UV detection at 210 and 330 nm. Rutin was not detected among the components of the syrup.     

High-performance liquid chromatography coupled to mass spectrometry for studying new pharmaceutical entities

The review covers the aspects of the use of high-performance liquid chromatography coupled to mass spectrometry for studying new pharmaceutical entities. Attention is paid mainly to pharmacokinetic investigations. Different methods of sample preparation and approaches to minimize the duration of the analysis are discussed.     

Traceability without uncertainty: current situation in the pharmaceutical industry

The current situation in the pharmaceutical industry is discussed, when the traceability of measurement (analytical) results to certified values of pharmacopoeial reference standards is required, without evaluating their uncertainties. It is shown that the evaluation of measurement uncertainty is necessary for understanding the level of confidence of the analytical results and their comparability, particularly during preparation and characterisation of the reference standards.Papers published in this section do not necessarily reflect the opinion of the Editors, the Editorial Board and the Publisher. Apart from exceptional circumstances, they are not submitted to the usual referee procedure and go essentially unaltered.     

Study on polymerization of the pharmaceutical substances isohexenylnaphthazarins

Polymerization of naturally occurring isohexenylnaphthazarins (IHN), such as alkannin, shikonin (A/S) and their derivatives, which are potent pharmaceutical substances, significantly affects their use in pharmaceuticals, cosmetics and as food colorants, because it leads to reduction of the lustre of their red coloration, a decrease in their solubility and reduces the active monomeric IHN derivatives. In the present study, the influence of several crucial variables (processing and storage) was experimentally investigated on IHN polymerization by size exclusion chromatography (SEC). Temperature and solvent polarity increased significantly the concentration of hydroxynaphthoquinone (HNQ) polymers, while air and light exposure conditions did not significantly affect IHN polymerization. Low temperatures are proposed for all processes of industrial production of pharmaceutical preparations containing IHN and HNQ. An optimization of the industrial conditions used for the preparation of pharmaceutical and cosmetic preparations containing IHN, maximizing the active monomeric IHN fraction, was performed.     

Some applications of bonded-phase high-performance liquid chromatography to the analysis of pharmaceutical formulations

Chromatographic procedures are presented for the determination of guaiphenesin, phenylephrine hydrochloride, phenylpropanolamine hydrochloridfe, pholcodine, methyl and propyl 4-hydroxybenzoates, and tyrothricin in some pharmaceutical products. An investigation of the contamination of lozenges with aspirin, paracetamol, phenacetin, prednisone and prednisolone is reported, together with the preparation of a novel bonded weak cation-exchange packing used.     

Simultaneous spectrophotometric determination of fat-soluble vitamins in multivitamin pharmaceutical preparations

A spectrophotometric method is proposed for the simultaneous determination of vitamins A, D and E in multivitamin pharmaceutical preparations. This is based on multiple linear regression. Most vitamins are directly extracted from the preparations into n-hexane. Microen-capsulated vitamin A preparations require pretreatment of de-encapsulation before the vitamin is extracted. The wavelength range to be used for each preparation and the optimum spectral mode (absorbance or first-derivative) has been chosen in order to assure correct quantitation and avoid interferences from other absorbing species also extracted by n-hexane. The results obtained were validated by simultaneous HPLC analyses for accuracy and precision.     

Kinetics of oil saponification by lead salts in ancient preparations of pharmaceutical lead plasters and painting lead mediums

Lead soaps can be found in archaeological cosmetics as well as in oil paintings, as product of interactions of lead salts with oil. In this context, a better understanding of the formation of lead soaps allows a follow-up of the historical evolution of preparation recipes and provides new insights into conservation conditions. First, ancient recipes of both pharmaceutical lead plasters and painting lead mediums, mixtures of oil and lead salts, were reconstructed. The ester saponification by lead salts is determined by the preparation parameters which were quantified by FT-IR spectrometry. In particular, ATR/FT-IR spectrometer was calibrated by the standard addition method to quantitatively follow the kinetics of this reaction. The influence of different parameters such as temperature, presence of water and choice of lead salts was assessed: the saponification is clearly accelerated by water and heating. This analysis provides chemical explanations to the historical evolution of cosmetic and painting preparation recipes.     

Polymeric gels and hydrogels for biomedical and pharmaceutical applications

Hydrogels are formed when a three‐dimensional polymeric network is loosely crosslinked. They are swollen by water but not dissolved in it. Hydrogels may display reversible sol–gel transitions, induced by changes in the environmental conditions such as temperature, pH, ionic strength, phase separation, wave length of light, crystallinity, etc. Hydrogel is described as smart or intelligent when sharp transition is induced by small change in such conditions. For the shape‐memory hydrogels, reversible change in shape may also be induced by such stimuli. The preparation and applications of the molecularly imprinted polymeric hydrogels (MIPs) are illustrated by a few examples. The use of shape sensitive hydrogels in microfluidic is mentioned. Application of hydrogels for chronobiology and chronotherapy is outlined. The conversion of hydrogels into aerogels and their respective properties is discussed. Copyright © 2009 John Wiley & Sons, Ltd.     

Electrophoretic and gas-chromatographic analysis of an Afobazol pharmaceutical preparation

Procedures for determining 5-ethoxy-2-[2-(morpholino)ethylthio]benzimidazole dihydrochloride, an active component of the Afobazol medicinal preparation, and its potential impurities, 5-ethoxybenzimidazol-2-thione and N-(2-chloroethyl)morpholine hydrochloride by capillary zone electrophoresis in the range 2.0 × 10^?5 to 2.0 × 10^?3 M and ligand-exchange capillary electrophoresis in the range 1.0 × 10^?5 to 5.0 × 10^?3 M are developed. The optimum conditions for the separation and determination of these analytes using a quartz capillary tube are found. The reliability of the results obtained by capillary electrophoresis was confirmed by gas chromatography with a mass-selective detector.     

Advanced porous organic materials for sample preparation in pharmaceutical analysis

The development of novel sample preparation media plays a crucial role in pharmaceutical analysis. To facilitate the extraction and enrichment of pharmaceutical molecules in complex samples, various functionalized materials have been developed and prepared as adsorbents. Recently, some functionalized porous organic materials have become adsorbents for pharmaceutical analysis due to their unique properties of adsorption and recognition. These advanced porous organic materials, combined with consequent analytical techniques, have been successfully used for pharmaceutical analysis in complex samples such as environmental and biological samples. This review encapsulates the progress of advanced porous materials for pharmaceutical analysis including pesticides, antibiotics, chiral drugs, and other compounds in the past decade. In addition, we also address the limitations and future trends of these porous organic materials in pharmaceutical analysis.     

High-speed ion-pair partition chromatography in pharmaceutical analysis.

Ion-pair chromatography offers attractive possibilities in pharmaceutical analysis. The specificity of the separation systems can be varied over a wide range by appropriate selection of the stationary phase. The choice of a suitable counter-ion can also drastically improve the detection limit, permitting the determination of drug substances in low dosage and possibly of by-products or breakdown products. Ion-pair chromatography of tropane and ergot alkaloids has been investigated using picrate as counter-ion. Alumina, Kieselguhr and various grades of silica gel have been tested as supports. Partition properties studied in a batch procedure have been compared with the actual chromatographic conditions. Columns (10 cm) filled with silical gel (particle size, 5 mum; pore size, 1000 A) show the best performance in the separation of hyoscyamine, scopolamine and ergotamine as picrate ion-pairs. Close control of pH and temperature is essential for reproducible separations. Improvements in detection limits between 100 and 300 times have been observed with these systems. Ion-pair extractions of these alkaloids from dosage forms can be used for sample preparation prior to injection on the the column. This provides an added degree of selectivity and sensitivity.     

Polymorphic analysis of a pharmaceutical preparation by NIR spectroscopy

A method for the characterization and determination of the crystalline from present in the amorphous miokamycin of a pharmaceutical preparation using near-infrared spectroscopy (NIRS) is proposed. The study leading to the development of the proposed method involved both qualitative (classification by residual variance analysis) and quantitative aspects (the determination of both total miokamycin and its crystalline form using multivariate calibration). Samples containing less than 5% of the total amount of miokamycin in its crystalline form can be accurately classified. Partial least-squares regression (PLSR) allows low contents of the crystalline form to be determined with absolute errors less than 1.5%, which is comparable to the limit of detection of the X-ray diffraction technique used as reference. Also, the total miokamycin content is determined by NIRS with errors less than 1%. The simplicity, expeditiousness and robustness of the proposed method make it an effective tool for determining both total and crystalline miokamycin in solid dosage forms.     

Rapid accurate mass desorption electrospray ionisation tandem mass spectrometry of pharmaceutical samples

Desorption electrospray ionisation (DESI) has been successfully combined with a hybrid quadrupole time-of-flight mass spectrometer to provide mass spectra and product ion mass spectra of active ingredients formulated in pharmaceutical tablets, gels and ointments. Accurate mass data has been obtained from the DESI mass spectra and of the product ion fragments of selected ions, greatly enhancing the selectivity and information content of the experiment. This accurate mass information only takes seconds to acquire since the DESI technique does not require any sample preparation or extraction prior to mass analysis.     

Chromatographic analysis of penicillins in pharmaceutical formulations and biological fluids

Natural penicillin (benzylpenicillin) is the oldest antibiotic observed by Alexander Fleming in 1928. To broaden its spectrum of activity, natural penicillin was modified, giving rise to a group of antibiotics under the name 'penicillins'. Although an increasing number of bacteria appear to be resistant to them, penicillins are used to treat a variety of bacterial infections including Gram-positive, Gram-negative aerobic and anaerobic bacteria. Consequently, they are widely used in human and veterinary medicine to prevent and treat diseases. This review covers the analytical methodologies, mainly chromatographic, employed to the penicillins determination in pharmaceutical formulations, biological fluids and in production-scale fermentations reported in the literature. Results of published assays are comparatively presented focusing on sample preparation regarding isolation and purification, chromatographic conditions and method validation. Information on chemical structure, spectrum of activity and action mechanism of common penicillins has also been given.     

Spectral analysis of pharmaceutical formulations prepared according to ancient recipes in comparison with old museum remains

A study of the composition of the remains of ancient ointments from museums was undertaken to enable understanding of the preparation techniques. Comparison of ancient recipes from different historical periods and spectroscopic characteristics of inorganic and/or organic remains recovered in museum vessels enabled preparation of ancient pharmaceutical–cosmetic formulations. Farmacopea Augustana by Occo was one the most important books studied for the 14 formulations prepared in the laboratory. Three formulations are discussed in detail and raw materials and new preparations were proposed for ozone ageing. The most important micro Raman results are discussed. The spectra of the raw materials lipids, beeswax, and resins are discussed; beeswax and pig suet (axŭngia) Raman spectra were found to be similar, but different from those of the aged oils. SERS was applied to ancient ointments and galbanum and the Raman spectra are reported and discussed for the first time.     

Fluorimetric determination of danthron in pharmaceutical tablets and in urine

A simple, rapid determination is reported for danthron (1,8-dihydroxyanthraquinone) in pharmaceutical tablets. In a flow-injection system, danthron is reduced by sodium dithionite in $\text{1}\text{1}$ methanol/borate buffer to give a fluorescent complex. Linearity ranges from 30 μg ml^?1 to below 0.1 μg ml^?1. In urine samples, danthron is separated from other fluorescing species by reversed-phase high-performance liquid chromatography before its reduction by dithionite in a post-column reactor. Urine preparation requires no extraction. Spiked urine samples were studied in the working range of 0.02–2.0 μg ml^?1 danthron.     

Spectrophotometric determination of certain vicinal dihydroxybenzene derivatives in pharmaceutical preparations.

A simple, rapid and sensitive spectrophotometric method for the assay of certain adrenergic drugs, [pyrocatechol (PC), levodopa (LD), methyldopa (MD) and dopamine (DP)] is described. The method involves the oxidation of o-dihydroxybenzene derivatives by K2CrO4 followed by oxidative coupling with sulfanilic acid (SPA), leading to the formation of a red or violet colored product having maximum absorbance at 490-495 nm for LD, MD and DP or at 560 nm for PC. This method has been successfully applied to the determination of LD, MD and DP in tablets and injections of pharmaceutical preparation. The common excipients do not interfere with the proposed method. A statistical comparison of these results with those of a reported method shows good agreement and indicates no significant difference in precision.     

Application of micellar electrokinetic chromatography to the quality control of a pharmaceutical preparation containing three bronchodilators

Theophylline(1,3-dimethylxanthine), dyphylline [7-(2,3-dihydroxypropyl)theophylline] and proxyphylline [7-(beta-hydroxypropyl)theophylline] are three bronchodilators administered jointly in a single pharmaceutical preparation used against asthma. A micellar electrokinetic chromatography (MEKC) method for their resolution using a background electrolyte consisting of 20 mM tetraborate at pH 8.5 and 100 mM sodium dodecyl sulfate is proposed. The method was used to determine the three active principles in a pharmaceutical preparation. The small amount of sample required and the expeditiousness of the procedure allow content uniformity to be determined in individual tablets. The values of the validation parameters for the method (viz. selectivity, linearity, accuracy, precision, limit of detection, limit of quantitation and robustness) are reported. A complete factor design (2(3)x2) including pH, the surfactant concentration and the ionic strength of the background electrolyte as factors was used to estimate robustness. Based on the results, the method is robust enough for quantitation purposes.