Contribution to the Development and Validation of a High Performance Liquid Chromatography by the Uv Detection Method for Isoniazid and Omeprazole Determination (original) (raw)
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Analytica Chimica Acta, 1987
Isoniazid in solutions of tablets was separated by thin-layer chromatography (TLC). The portion of the precoated plate carrying the isoniazid spot was cut out and the coating was scraped off into water. The isoniazid was quantified in the solution, without separation of suspended adsorbent, by second-derivative spectrophotometry, which eliminated the background in the zero-order spectra. Relative standard deviations (n = 5) were <I%. Results obtained for commercial tablets were in good agreement with those given by a liquid-chromatographic method.
2020
A simple method using HPLC system for the quantification of Isoniazid, in a fixed-dose combination (FDC) of anti-tuberculosis drug product wasdeveloped and validated. The chromatographic separation of Isoniazid (INH) was carried out using Waters Symmetry C8 column (150× 4.6 mm: Particle size: 5 μm), UV detection at 262 nm, and anisocratic system with composed of mobile phase of Phosphate buffer solution (pH 6.8)and Acetonitrile in the ratio of 980:20,at a flow rate of 1.0 mL/min. The retention time of Isoniazid was about 3.8 minutes.
A Sensitive HPLC Method for Determination of Isoniazid in Rat Plasma, Brain, Liver and Kidney
Journal of Chromatography & Separation Techniques, 2012
A simple and rapid reverse phase high performance liquid chromatography (RP-HPLC) method was developed and validated for quantitative determination of Isoniazid (INH) in plasma, brain, liver and kidney samples and in solid lipid nanoparticles (SLNs). Isoniazid was analyzed by using a reverse phase column (Waters, Symmetry shield RP-18, 4.6 mm x 150 cm, 5 microns), with mobile phase consisting of 0.1 M phosphate buffer, pH 5 (pH adjusted with ortho phosphoric acid) and methanol and the detection was made at 254 nm using Photo Diode Array detector at a temperature of 30°C (sample 4°C). The retention time for INH was around 3.5 minutes. The calibration curves were linear (r 2 0.9998) over a concentration range from 250 ng to 25,000 ng/mL. Limit of detection (LOD) was 150 ng/mL and the Limit of quantitation (LOQ) was 200 ng/mL for plasma and tissue homogenates (brain, liver and kidney). Intra and inter-day variability's (RSD) for extraction of INH from plasma and other tissue homogenates were less than 5% and accuracy was ± 5%. The results established selectivity and suitability of the method for pharmacokinetic studies of INH from INH SLNs.
ACTA Pharmaceutica Sciencia
To develop two new spectrophotometric methods for the analysis of isoniazid in bulk form and tablets. The methods involved condensation of isoniazid with salicylaldehyde and diazo coupling with diazotized p-nitroaniline. Critical factors were optimised; evidence for new product formation, selection of analytical wavelengths, temperature and time and solvent for dilution. Validation was carried out according to ICH guidelines. The new methods were used for isoniazid tablets. Isoniazid formed an imine and azo adduct readily with the two reagents at 30 ⁰C after 5 and 20 mins, and determined at 405 and 420 nm, respectively. Low LODs were obtained for the two methods and recoveries were generally above 98%. The methods were successfully adopted for the assay of isoniazid in tablets and there were no significant differences in the contents when compared with the official titrimetric method of analysis. The methods could find application as in-process method in pharmaceutical industries.
Improved high performance liquid chromatographic analysis of omeprazole in human plasma
A simple high-performance liquid chromatographic method was developed for the determination of omeprazole in human plasma. Omeprazole and the internal standard, chloramphenicol, were extracted from alkalinized plasma samples using dichloromethane. The mobile phase was 0.05 M Na 2 HPO 4 -ACN (65:35, v/v) adjusted to pH 6.5. Analysis was run at a flow rate of 1.0 ml/min at a detection wavelength of 302 nm. The method was specific and sensitive with a detection limit of 2.5 ng/ml at a signal-to-noise ratio of 4:1. The limit of quantification was set at 5 ng/ml. The calibration curve was linear over a concentration range of 5 -1280 ng/ml. Mean recovery value of the extraction procedure was about 96%, while the within and between day coefficient of variation and percent error values of the assay method were all less than 14%.
Dhaka University Journal of Pharmaceutical Sciences, 2010
A Simple RP-HPLC method with UV detection has been validated to determine omeprazole concentrations in human serum and urine samples. The mobile phase consisted of a mixture of potassium dihydrogen phosphate buffer (pH 7.2 ± 0.05; 0.2 M) and acetonitrile (70:30, v/v), pumped at a flow rate of 1.0 ml/min through the C-8 column at room temperature. Peaks were monitored by UV absorbance at 302 nm at a sensitivity of 0.0001. The developed method was selective and linear for omeprazole concentrations ranging between 5 to 1000ng/ml for serum samples and 1 to 100μg/ml for urine samples. The recovery of omeprazole ranged from 95.68 to 99% and 95.54 to 99.8% for the serum and urine samples respectively. The limit of quantitation (LOQ) of omeprazole was 5 ng/ml. The intraday accuracy ranged from 93.54 to 104.38% and 100.55 to 103.48% for the serum and urine respectively. The interday accuracy varied from 97.61 to 113.95% and 97.42 to 109.97% for the serum and urine respectively. For the LOQ, ...
Analytical Letters, 1999
A new selective high-performance liquid chromatography (HPLC) method with UV detection for the determination of the investigational triazole voriconazole in human plasma by using acetonitrile precipitation followed by reverse-phase HPLC on a C 18 column was compared with a simple agar well diffusion bioassay method with Candida kefyr ATCC 46764 as the assay organism. Pooled plasma was used to prepare standard and control samples for both methods. The results of analyses with spiked serum samples (run as unknowns) were concordant by the bioassay and HPLC methods, with expected values being obtained. HPLC demonstrated an improved precision (3.47 versus 12.12%) and accuracy (0.81 versus 1.28%) compared to those of the bioassay method. The range of linearity obtained by both methods (from 0.2 to 10 g/ml for HPLC and from 0.25 to 20 g/ml for the bioassay) includes the range of concentrations of voriconazole (from 1.2 to 4.7 g/ml) which are considered clinically relevant. Although either methodology could be used for the monitoring of patient therapy, the smaller variability observed with HPLC compared to that observed with the bioassay favors the use of HPLC for pharmacokinetic studies.
A simple reversed-phase high performance liquid chromatography has been developed and employed for the analysis of Omeprazole and its related substances in bulk material and commercial dosage forms. A gradient elution of filtered sample was performed on Zorbax XDB C8 (150 x 4.6), 5µ column with Glacine buffer (pH -8.8) as a mobile phase-A, Acetonitrile : Methanol (83:17) as a mobile phase-B and UV detection at 302 nm. Mobile phase was delivered at flow of 1.2 mL/min and at maintaining the column temperature at 25ºC, quantification was achieved with reference to the external standards. The active ingredientomeprazole was successfully separated from its all related substances, including process impurities and other possible impurities of oxidation and decomposition. The excipients did not interfere with the determination of omeprazole and its related compound in commercial dosage formulations. The method was rapid, simple, accurate and reproducible. It was not only successfully employed for the assay of omeprazole in bulk material and pharmaceutical dosage forms but also for the determination of its related substances. A statistical design of experiments was used for the robustness evaluation of HPLC analysis method. All results were acceptable and confirmed that the method is suitable for its intended use.
Chromatographia, 1990
A rapid, simple, and accurate method was developed for the determination of isoniazid and its metabolites (isonicotinic acid, acetylisoniazid and isonicotinylglycine) in urine by high-performance liquid chromatography. Urine is diluted with the mobile phase. After centrifugation, an aliquot of the supernatant is injected into the chromatograph. Isoniazid and its metabolites are separated by reversed-phase ionpairing chromatography with a mobile phase containing propanesulfonate and detected by fluorometry using postcolumn derivatization at high temperature (150 ~ with hydrogen peroxide. The method was applied to the analysis of urine from patients receiving isoniazid therapy.
2014
New, simple and cost effective spectrophotometric methods have been developed for the quality assessment of isoniazid (INH), in bulk and in pharmaceutical formulations by using novel reagents. The proposed methods involve the utility of ethyl 2-[(E)-(4-hydroxyphenyl) diazenyl]-3-oxobutanoate and benzil as novel reagents for the determination of INH. Developed methods are based on the condensation reaction of INH with reagents to give orange colored chromogen with an absorption band at 454 nm (for method A) and 436 nm (for method B). The applicability of these methods is demonstrated by the determination of the studied drug in commercial tablets and the results are statistically evaluated. The new procedures described in this paper are fast, convenient and have the novelty of carrying out the quantitative determination of INH in pure and in pharmaceutical formulation.