Development of a simple UV-spectrophotometric method for the determination of lansoprazole and study of its degradation profile

A UV-spectrophotometric method is described for the determination of lansoprazole (LAN). The method is based on the measurement of the absorbance of LAN solution in acetonitrile at 281 nm. The system obeyed Beer's law over the concentration range of 1.25-25.0 µg/mL. The degradation behavior of LAN was investigated under dry heat treatment, UV-degradation, acid hydrolysis, alkali hydrolysis and oxidation; and found to degrade extensively under acid hydrolysis, alkali hydrolysis and oxidation. The method was applied to the determination of LAN in capsule and the results were statistically compared with those of the reference method by applying Student's t-test and F-test.

Studies on the development of spectrophotometric method for the determination of haloperidol in pharmaceutical preparations

A spectrophotometric method based on the formation of ion-pair complex between haloperidol and eriochrome black T (EBT) at pH 1.85 has been described. The formed complex was extracted quantitatively into chloroform and measured at 510 nm. Infra red (IR) studies were performed to confirm the formation of ion-pair complex. Beer's law was obeyed in the concentration range of 2.0-9.0 µg mL-1 with molar absorptivity of 2.67 × 10(4) L mol-1 cm-1. The detection limit was found to be 0.18 µg mL-1. Statistical comparison of the results of the proposed method with those of the reference method shows excellent agreement and indicates no significant difference in accuracy and precision.

A validated method using RP-HPLC for quantification of reserpine in the Brazilian tree Rauvolfia sellowii Müll. Arg. (Apocynaceae)

This study describes a simple, fast and reproducible method using RP-HPLC-UV, in a gradient system, for quantification of reserpine in Rauvolfia sellowii stem bark. The analysis were carried out on a C18 column; mobile phase was water and acetonitrile, and separations were carried out in 10 min, flow rate of 1.0 mL min-1, 25 ºC and 268 nm. The validation data showed that the method was specific, accurate, precise and robust. Results were linear over a range of 0.625-40.0 μg mL-1, and the mean recovery was 95.1%. The amount of reserpine found in the dried stem bark was 0.01% (m/m).

Sensitive method for determination of piplartine, an alkaloid amide from Piper species, in rat plasma samples by liquid chromatography-tandem mass spectrometry

Piplartine (PPTN) is an alkaloid amide found in Piper species that presents different activities. PPTN determination in rat plasma is necessary to better understand its biological effects. The aim of this study was to develop a sensitive LC-MS/MS method for the determination of PPTN in rat plasma. The performance criteria for linearity, sensitivity, precision, accuracy, recovery, and stability have been assessed and were within the recommended guidelines. The validated method proved to be suitable in a pilot study of PPTN kinetic disposition in rat plasma after a single intraperitoneal dose, and represents an appropriate tool to further pharmacokinetic studies.

Synthesis of indium tin oxide nanoparticles by a nonhydrolytic sol-gel method

Indium tin oxide nanoparticles were synthesized in two different sizes by a nonhydrolytic sol-gel method. These powders were then transformed into ITO via an intermediate metastable state at between 300 and 600 ºC. The presence of characteristic O-In-O and O-Sn-O bands at 480 and 670 cm-1 confirmed the formation of ITO. The X-ray diffraction patterns indicated the preferential formation of metastable hexagonal phase ITO (corundum type) as opposed to cubic phase ITO when the reflux time was less than 3 h and the heat treatment temperature was below 600 ºC. Particle morphology and crystal size were examined by scanning electron microscopy.

Romp as a versatile method for the obtention of differentiated polymeric materials

Ring Opening Metathesis Polymerization (ROMP) of cyclic olefins is a powerful transition metal-catalyzed reaction for syntheses of polymers and copolymers. The key feature of this reaction is the [2+2]-cycloaddition mechanism, with retention of the olefinic unsaturation in the polymer chain and occurrence of living polymerization. With the development of metal-carbene type catalysts for this process, many addressed polymeric materials have been successfully prepared to be employed in several fields of the science and technology. This review summarizes recent examples of syntheses of polymers with amphiphilic features such as block, graft, brush or star copolymers; as well syntheses of biomaterials, dendronized architectures, photoactive polymers, cross-linked or self-healing materials, and polymers from renewed supplies.

Chlorophenols in tap water from wells and surface sources in Rio de Janeiro, Brazil: method validation and analysis

Two analytical methods were validated for determination of trichlorophenols, tetrachlorophenols and pentachlorophenol in drinking water. Limits of quantification were at least ten times lower than maximum permissible levels set by the Brazilian legislation, which are 200 ng mL-1 for 2,4,6-trichlorophenol and 9 ng mL-1 for pentachlorophenol. Chlorophenol levels were determined in tap water collected in the Municipality of Rio de Janeiro. 2,4,6-Trichlorophenol residues were detected in 36% of the samples, varying from 0.008 to 0.238 ng mL-1. All other analytes were below the limit of quantification. The validated methods showed to be suitable for application in routine quality control.

Set-up of a method using LC-UV to assay mometasone furoate in pharmaceutical dosage forms

A reliable method using LC-UV to assay mometasone furoate (MF) in creams or nasal sprays using the same chromatographic conditions was set up. Methanol:water 80:20 (v/v) (1.0 mL min-1) was used as mobile phase. MF was detected at 248 nm and analyzed in a concentration range from 1.0 to 20.0 µg mL-1. The method provided acceptable theoretical plates, peak simmetry, peak tailing factor and peak resolution a short run (5 min). The method showed specificity, good linearity (r = 0.9999) and the quantification limit was 0.379 µg mL-1. Furthermore, the method was precise (RSD < 2.0%), accurate (recovery > 97%) and robust.

Development of a UV/Vis spectrophotometric method for analysis of total polyphenols from Caesalpinia peltophoroides Benth

Caesalpinia peltophoroides is a domesticated tree found in Brazil. It was necessary to develop an analytical method to determine the content of total polyphenols (TP) in this herbal drug. The pre-analytical method was standardized for analysis time, wavelength, and the best standard to use. The optimum conditions were: pyrogallol, 760 nm, and 30 min respectively. Under these conditions, validation by UV/Vis spectrophotometry proved to be reliable for TP of the crude extract and semipurified fractions from C. peltophoroides. Standardization is required for every herbal drug, and this method proved to be linear, precise, accurate, reproducible, robust, and easy to perform.

Development and validation of a novel stability indicating RP-UPLC method for simultaneous determination of nizatidine, methylparaben and propylparaben in oral liquid pharmaceutical formulation

A selective and accurate stability-indicating gradient reverse phase ultra performance liquid chromatographic method has been developed and validated for the simultaneous determination of nizatidine, methylparaben and propylparaben in pharmaceutical oral liquid formulation. The separation was achieved on Acquity UPLC TM HSS T3 1.8 µm column by using mobile phase containing a gradient mixture of solvent A (0.02 Mol L-1 KH2PO4, pH 7.5) and B (60:40 v/v mixture of methanol and acetonitrile) at flow rate of 0.4 mL min-1. Drug product was exposed to the stress conditions of oxidative, acid, base, hydrolytic, thermal and photolytic degradation. The developed method was validated as per international ICH guidelines with respect to specificity, linearity, accuracy, precision and robustness.

Stability indicating HPLC method for simultaneous determination of moxifloxacin hydrochloride and ketorolac tromethamine in pharmaceutical formulations

A simple, RP-HPLC method was established for determining moxifloxacin and ketorolac in pharmaceutical formulations. Moxifloxacin, ketorolac and their degradation products were separated using C8 column with methanol and phosphate buffer pH 3.0 (55:45 v/v) as the mobile phase. Detection was performed at 243 nm using a diode array detector. The method was validated using ICH guidelines and was linear in the range 20-140 µg mL-1 for both analytes. Good separation of both the analytes and their degradation products was achieved using this method. The developed method can be applied successfully for the determination of moxifloxacin and ketorolac.

Development and validation of a High Performance Liquid Chromatographic method for determination of etoposide in biodegradable polymeric implants

A method using HPLC-UV was developed and validated for the determination of etoposide incorporated into polycaprolactone implants. The method was carried out in isocratic mode using a C18 column (250 x 4.6 mm; 5 µm), at 25 ºC, with acetonitrile and acetic acid 4% (70:30) as mobile phase, a flow rate of 2 mL/min, and UV detection at 285 nm. The method was linear (r² > 0.99) over the range of 5 to 65 µg/mL, precise (RSD < 5%), accurate (recovery of 98.7%), robust, selective regarding excipient of the sample, and had a quantitation limit equal to 1.76 µg/mL. The validated method can be successfully employed for routine quality control analyses.

Indirect spectrophotometric method for determination of captopril using Cr(VI) and diphenylcarbazide

A spectrophotometric method for the indirect determination of captopril (CP) in pharmaceutical formulations is proposed. The proposed procedure is based on the oxidation of captopril by potassium dichromate and the determination excess oxidant on the basis of its reaction with diphenylcarbazide (DPC). Under the optimum conditions, a good linear relationship (r = 0.9997) was obtained in the range of 0.08-3.5 µg mL-1. The assay limits of detection and quantitation were 0.024 and 0.08 µg mL-1, respectively. The results obtained for captopril determination in pharmaceuticals using the proposed method and those obtained with the US Pharmacopoeia method were in good agreement at the 95% confidence level.

A validated HPLC analytical method for the analysis of solasonine and solamargine in in vitro skin penetration studies

To assess topical delivery studies of glycoalkaloids, an analytical method by HPLC-UV was developed and validated for the determination of solasonine (SN) and solamargine (SM) in different skin layers, as well as in a topical formulation. The method was linear within the ranges 0.86 to 990.00 µg/mL for SN and 1.74 to 1000.00 µg/mL for SM (r = 0.9996). Moreover, the recoveries for both glycoalkaloids were higher than 88.94 and 93.23% from skin samples and topical formulation, respectively. The method developed is reliable and suitable for topical delivery skin studies and for determining the content of SN and SM in topical formulations.

Improved method to obtain pfaffic acid as a marker for quality control

Pfaffic acid, a marker of Hebanthe eriantha (Brazilian ginseng), was first isolated in 1983 but is not yet commercially available. This lack of availability compromises the quality control of this plant and its derivatives. This paper proposes a process for pfaffic acid isolation from roots of H. eriantha at a purity suitable for analytical purposes. The steps involved in this process included extraction, hydrolysis, fractionation and purification by preparative HPLC. This process led to isolation of pfaffic acid with a chromatographic purity of 98.5% in a 0.25% yield from dried roots of H. eriantha; this yield is more than forty times higher than that of the current method in the literature.