Development of a high sensitivity RP-HPLC method and stress testing of imatinib mesylate 1 (original) (raw)
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A validated LC method for imatinib mesylate
… of pharmaceutical and …, 2003
An isocratic reversed-phase liquid chromatography method with UV detection has been developed for the purity evaluation of imatinib mesylate in bulk drug. The method is selective and is capable of detecting all process intermediates and other related compounds, which may be present at trace levels in the drug substance. The method was validated on a Symmetry Shield RP18 analytical column (150)/4.6 mm, 5 mm), mobile phase consisting of 30 mM sodium octane sulphonic acid in 10 mM aqueous KH 2 PO 4 (pH 2.5 with H 3 PO 4): MeOH in the ratio of 42:58 v/v. The flow rate was set at 1.0 ml/min and the column was maintained at room temperature. The injection volume was set to 10 ml and the detector was set at a wavelength of 237 nm. The method was validated in terms of system precision, method precision, linearity, accuracy, limit of detection and limit of quantification.
Development of Analytical Method for Imatinib Mesylate by Ultraviolet Spectroscopy
Asian Journal of Pharmaceutical and Clinical Research
Objective: A simple, selective, sensitive, specific, and spectrophotometric method has been developed for the detection of imatinib mesylate in pure form and formulations. Methods: The analytical condition was optimized for the drug, carried out as per the International Council for Harmonisation of Technical Requirements for Pharmaceuticals for Human Use guidelines. Results: The drug shows absorption at 232.0 nm and obeyed beers law in the wide concentration range from 0.5 to 4.0 μg/ml. The lower limit of detection was found to be 0.331 μg/ml and the limit of quantification to be 1.004 μg/ml. The regression equation was found to be y = 0.08x. The precision of the method was found to be 99.04%±0.527% and the percentage of drug recovered by this method is 100.13%±1.375%. Conclusion: The method is simple and suitable for determination for imatinib mesylate in pure and pharmaceutical preparation.
Journal of Chromatographic Science, 2010
A simple, selective, and sensitive liquid chromatographic method has been developed and validated for quantitative determination of Imatinib mesylate in rat serum. Efficient chromatographic separation has been performed on a Zorbax Extend (5 µm, 4.6 × 250 mm) double end-capped C 18 column using a mobile phase consisting of methanol and aqueous triethyl amine (pH 10.5; 1%, v/v) (60:40, v/v) in an isocratic mode at a flow rate of 1 mL/min. Simple and effective liquid-liquid extraction technique has resulted in consistent and high recoveries (90.32-95.86%) at all concentrations studied. The method has demonstrated linearity from 25 to 1600 ng/mL with a regression coefficient of 0.9995. Accuracy of the method is acceptable with intra-batch %bias between −2.34 to 3.42 and inter-batch %bias between −2.17 to 3.45. The method has demonstrated high sensitivity with lower limit of quantification of 25 ng/mL and excellent stability of Imatinib mesylate in serum. The method is found to be rapid, reliable, and suitable for in vivo pharmacokinetic study.
Validation of an HPLC Method for the Determination of Imatinib Mesylate in Pharmaceutical Dosage
Journal of Liquid Chromatography & Related Technologies, 2005
A simple HPLC method with fluorescence detection of ciprofloxacin in human plasma was developed and validated. After protein precipitation, chromatographic separation of ciprofloxacin in plasma was achieved at 35 8C with a C18 column and acetonitrile Á/phosphate mixture, pH 3, as mobile phase. Quantitative determination was performed by fluorimetry after excitation at 278 nm. The method was specific and validated with a limit of quantification of 41 ng/ml. The intra-and inter-day coefficients of variation were between 0.5 and 6.6% and accuracy between (/2.02 and 7.04%. Ciprofloxacin was stable in plasma for 40 days at (/20 8C and after three freezing-thawing cycles. The method has been applied in a bioequivalence study of two formulation of 500 mg ciprofloxacin. #
. Spectrophotometric Determination of Imatinib Mesylate
Two new, simple and effective colorimetric methods were developed for determination of Imatinib (mesylate) in pure and pharmaceutical formulations. Charge transfer (CT) interactions between Imatinib as electron donor and 2,3-dichloro-5,6,-dicyano-p-benzo quinone (DDQ) and chloranilic acid (CAA) as π-electron acceptors. The obtained charge-transfer complexes were measured at λ max 462 nm and 537 nm for DDQ and CAA in methylene chloride, respectively. Different variables affecting the reaction were studied and optimized. Under the optimum conditions, Beer's law was obeyed in the concentration range of the drug 0.25-3.50 mg/ 10 ml and 0.50-5.50 mg/ 10 ml upon using DDQ (0.4% w/v) and CAA (0.3% w/v), respectively, with correlation coefficients 0.996 and 0.998, respectively. The proposed methods showed good linearity, precision, reproducibility and the validity was assessed by applying the standard additions technique with mean percentage recovery 99.90 ± 1.36 in case of DDQ and 100.20 ± 0.91 in case of CAA.
Brazilian Journal of Pharmaceutical Sciences, 2020
Imatinib mesylate is a small molecule used in cancer therapy as a thyrosine kinase inhibitor. Dexketoprofen trometamol is a non-steroidal anti-inflammatory drug that has seen use in cancer therapy in combination with an anticancer drug to minimize tumor size and to reduce pain in patients. In the present study, imatinib mesylate and dexketoprofen trometamol were selected as potential model drugs to be used in combination. A new, simple and selective Ultra Performance Liquid Chromatography method was developed and validated to determine the drug substances in distilled water, in a pH 7.4 phosphate buffer and in Dulbecco's Modified Eagle Medium. The proposed method was developed using a BEH C-18 column with isocratic elution. A mixture of methanol:acetonitrile (80:20, v/v) and pH 9.5, 0.05 M ammonium acetate were (70:30, v/v) used as a mobile phase. Detection was carried out with a flow rate of 0.3 mL/min, a column temperature of 30°C and an injection volume of 20 µL. The method was validated considering linearity, accuracy, precision, specificity, robustness, detection limit and quantitation limit values, and was found to be linear in a range from 0.05 to 20.0 µg/mL for the three different media.
Visible Spectrophotometric Method Development and Validation of Imatinib in Bulk and Formulation
International Journal of Current Pharmaceutical Research, 2020
Objective: A new, simple, sensitive, precise and reproducible UV visible spectrophotometric method was developed for the determination of Imatinib in pharmaceutical formulations with alizarin. Methods: The method is based on formation of yellow-colored complex. The UV spectrum of Imatinib in methanol showed λ max at 431 nm. Beer’s law is valid in the concentration range of 10-70 μg/ml. This method was validated for linearity, accuracy, precision, ruggedness and robustness. Results: The method has demonstrated excellent linearity over the range of 10-70 μg/ml with regression equation y =0.013x-0.017 and regression correlation coefficient r2= 0.997. Moreover, the method was found to be highly sensitive with LOD (4.3μg/ml) and LOQ (13.07μg/ml). Conclusion: Based on results the proposed method can be successfully applied for the assay of Imatinib in various pharmaceutical dosage forms.
2010
Received on 12-05-2010 Accepted on 21-06-2010 A Simple and sensitive spectrophotometric method has been developed for the estimation of Imatinib mesylate in both pure and tablet dosage form. The proposed method is based on the measurement of light absorption in uv region in distilled water. The UV spectrum of Imatinib mesylate in distilled water showed λmax at 256 nm. Beer’s law is valid in the concentration range of 2-12 µg/ml. This method was validated for precision, accuracy, ruggedness and robustness. Statistical analysis proves that the method is reproducible and selective for the estimation of the said drug. Key Words: Spectrophotometry, Imatinib mesylate
Journal of Chromatography B, 2004
The aim of this study was to develop a rapid and sensitive HPLC method with UV detection for the estimation of imatinib from the plasma of patients with chronic myeloid leukemia (CML). The robustness of the method was checked by conducting first dose pharmacokinetics on blood samples from four patients who had been administered Gleevec (100 mg) in an oral dose. Samples were prepared in a simple and single step by precipitating the plasma proteins with methanol and injecting 50 l aliquot from supernatant was subjected for analysis. Assay was conducted using a C8 column (250 mm × 4.6 mm, 5 m particle size) under isocratic elution with 0.02 M potassium dihydrogen phosphate-acetonitrile (7:3, v/v) at a flow rate of 1 ml/min and detected using photodiode array at 265 nm. Calibration plots in spiked plasma were linear in a concentration range of 0.05-25 g/ml. The inter and intra-day variation of standard curve was <4% (R.S.D.). This method could be a simple and quick method for the estimation of imatinib from the patient's plasma.