Ultra-fast gradient LC method for omeprazole analysis using a monolithic column: assay development, validation, and application to the quality control of omeprazole enteric-coated pellets (original) (raw)
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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.
Asian Journal of Chemistry, 2015
Omeprazole is a widely used proton pump inhibitor prescribed for the treatment of dyspepsia, peptic ulcer disease, gastro esophageal reflux disease, laryngo pharyngeal reflux and Zollinger-Ellison syndrome. A new ultra performance liquid chromatographic (UPLC) method was developed and validated for the quantitative analysis of omeprazole in a capsule dosage form. The separation and analysis of the related drug in the presence of ondansetron as internal standard (IS) were performed on Waters UPLC BEH C18 column (50 mm × 2.1 mm i.d., 1.7 µm) using a mobile phase consisting of acetonitrile and 0.05 M H3PO4 (28:72 v/v). Flow rate of the used mobile phase was 0.28 mL/min. The retention time for omeprazole and internal standard was found to be 0.787 and 1.060 min, respectively. A calibration graph for omeprazole in the concentration range of 4-46 µg/mL was obtained by using peak area ratio of omeprazole and internal standard in their chromatogram obtained by the detection at 302 nm. In the method validation process, percent mean recovery and relative standard deviation was found as 101.6 % and 1.20 %, respectively. It was observed that the application of the newly developed UPLC method gave us successful results for the quantitative estimation of omeprazole in capsules.
Asian Journal of Pharmaceutical Research and Development
Omeprazole,13 a member of proton pump inhibitor, used for the treatment of peptic ulcers, it supresses gastric acid secretion by inhibiting H+/K+ ATPase. A new fundamental, rapid and sensitive HPLC method was developed for the assay of Omeprazole sodium for injection. It was validated according to ICH and FDA guidelines 2. The HPLC analysis was performed on Dionex ultimate 3000 system equipped with C-18 (150cm*4.6mm) 5µ column, with a mixture of ammonium acetate and acetonitrile buffer in the ratio 65:35 v/v as the mobile phase at the wavelength (λ) 305nm. The total run time was 8 minutes. The calibration curve was linear for 50-150% range of the analytical concentration of 40mg/ml, r2 was found to be 0.9998. The precision was calculated and % RSD was 0.1 % and the recovery of omeprazole was within the range of 98-102%. Validation parameters like robustness, solution stability studies, specificity and forced degradation studies were performed and found to be within acceptance limit...
Development and Validation of a RP‐HPLC Method to Quantify Omeprazole in Delayed Release Tablets
Journal of Liquid Chromatography & Related Technologies, 2007
An accurate, simple, reproducible, and sensitive liquid chromatographic method is developed and validated to quantitate acyclovir (ACV) in cross-linked chitosan microspheres produced by spray drying. The analysis is carried out using a reversed-phase C 18 column with UV-vis detection at 254 nm. The mobile phase is diluted with pure water and acetonitrile (95:5 v/v) at a flow-rate of 0.8 mL/min. The parameters used in the validation process are: linearity, range, quantitation limit, detection limit, accuracy, specificity precision, and ruggedness. The retention time of acyclovir is approximately 3.5 min with symmetrical peaks. The linearity in the range of 1-10 µg/mL presents a correlation coefficient of 0.9999. The chitosan and the tripolyphosphate in the formulation do not interfere with the analysis, and the recovery is quantitative. Results are satisfactory, and the method proves to be suitable to quantitate ACV in cross-linked chitosan microspheres.
Determination of omeprazole in bulk and injectable preparations by liquid chromatography
Journal of AOAC International
An accurate, simple, reproducible, and sensitive liquid chromatographic method was developed and validated for the determination of omeprazole in powder for injection and in pellets. The analyses were performed at room temperature on a reversed-phase C18 column of 250 x 4.6 mm id, 5 microm particle size. The mobile phase, composed of methanol-water (90 + 10, v/v), was pumped at a constant flow rate of 1.5 mL/min. Detection was performed on a UV detector at 301 nm. The method was validated in terms of linearity, precision, accuracy, and ruggedness. The response was linear in the range 32-48 microg/mL (r2 = 0.9976). The relative standard deviation values for intra- and interday precision studies were 1.22 and 1.56% for injectable and 2.13 and 2.45% for pellets, respectively. Recoveries ranged between 95.81 and 100.48%.
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%.
Scientia pharmaceutica, 2013
A simple, fast, and sensitive reversed-phase HPLC method with UV detection was developed for the quantitation of omeprazole and its eleven related compounds (impurities) in pharmaceutical formulation using the Thermo Accucore C-18 (50 mm × 4.6 mm, 2.6 μm) column. The separation among all the compounds was achieved with a flow rate of 0.8 mL min(-1) employing a gradient program of mobile phase A [0.08 M glycine buffer pH 9.0: acetonitrile; 95:05 (v/v)] and mobile phase B [acetonitrile: methanol; 65:35 (v/v)]. The chromatographic detection was carried out at a wavelength of 305 nm. The method was validated for specificity, linearity, and recovery. The huskiness of the method was determined prior to validation using the Design of Experiments (DOE). The ANOVA analysis of DOE with a 95% confidence interval (CI) confirmed the buffer pH of mobile phase A (p <0.0001) and column temperature (p<0.0001) as significant Critical Method Parameters (CMPs).
Journal of Chromatography B, 2006
Bioanalytical methods using liquid/liquid extraction (LLE) and liquid chromatography with electrospray tandem mass spectrometry (LC-MS/MS) are widely used. The organic extracts need to be evaporated and reconstituted, hampering further improvement of throughput and automation. In this study, we demonstrated a novel approach of eliminating these two steps in 96-well LLE by using hydrophilic interaction chromatography with MS/MS (HILIC-MS/MS) on silica column with high organic/low aqueous mobile phase. Omeprazole, its metabolite 5-OH omeprazole, and internal standard desoxyomeprazole, were extracted from 0.05 ml of human plasma using 0.5 ml of ethyl acetate in a 96-well plate. A portion (0.1 ml) of the ethyl acetate extract was diluted with 0.4 ml of acetonitrile and 10 l was injected onto a Betasil silica column (50 mm × 3.0 mm, 5 m) and detected by API 3000 and 4000 with (+) ESI. Mobile phase with linear gradient elution consists of acetonitrile, water, and formic acid (from 95:5:0.1 to 73.5:26.5:0.1 in 2 min). The flow rate was 1.5 ml/min with total run time of 2.75 min. The method was validated for a low limit of quantitation at 2.5 ng/ml for both analytes. The method was also validated for specificity, reproducibility, stability and recovery. Lack of adverse matrix effect and carry-over was also demonstrated. The inter-day precision and accuracy of the quality control samples at low, medium and high concentration levels were <4.
IJEAST, 2022
A simple and fast flow-injection method for the determination of omeprazole in pharmaceutical preparations is proposed. Detection of the drug is based on the measurement of the absorption signals for the product resulting from the oxidation of omeprazole with N-bromosuccinimide in acidic medium. A flow rate of 0.5 ml/min was pumped and active material was detected at 370 nm. Limit of detection (LOD) and limit of quantitation (LOQ) were calculated to be 2.0 and 6.5 μg/ml, respectively. No interference was observed from common pharmaceutical additives. The method was successfully applied to the assay of omeprazole in capsule preparations and in spiked human plasma. The results were statistically compared with those of the official high-performance liquid chromatography (HPLC) method of the USP by applying Student's t-test and F-test.
A Simple HPLC Method for the Determination of Omeprazole in Vitro
International Journal of Pharmaceutical Chemistry, 2013
Omperazole was used for the treatment of stomach and gastroesophageal reflux disease. Omperazole was used administered in the form of oral dose as independent or combination form. Â Presnt study was carried out to develop and validate a simple HPLC methtod of determination of omeprazole in vitro. Â Mobile phase empolyed was acetonitrile: phosphate buffer (65: 35), pH 6.8 and C 18 column was used. UV detector was used using 300nm eluted with the mobile phase 1.0 mint/ml.