HPLC METHOD DEVELOPMENT, VALIDATION, AND FORCED DEGRADATION FOR SIMULTANEOUS ANALYSIS OF OXYCODONE AND NALTREXONEIN PHARMACEUTICAL DOSAGE FORM

A simple, precise and stability-indicating RP-HPLC method was developed for simultaneous quantification of oxycodone (OXCD) and naltrexone (NTRX) in combined dosage form. The developed method was validated with respect to precision, linearity, accuracy, robustness, ruggedness, sensitivity and solution stability. The method was developed with ammonium di hydrogen phosphate buffer (pH 5.0) and acetonitrile in a ratio of 55:45 (v/v) as mobile phase at a flow rate of 1.0 mL/minute over Intersil ODS C18 column (250 mm × 4.6 mm×5μ).The UV detection wavelength was fixed at 235 nm. The column temperature was maintained at ambient temperature. The method showed good linearity with correlation coefficient values of 0.9990 and 0.9994 for OXCD and NTRX. The percent recoveries of the two drugs found within the limits of 98.0–102.0%. The LOQ concentrations of OXCD and NTRX are 0.625 μg/ mL and 0.075 μg/mL, respectively. The LOD concentrations of OXCD and NTRX are 0.3125 μg/mL and 0.0375 μg/mL, respectively. According to ICH guidelines forced degradation study was validated.

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A new simple RP-HPLC Method development, Validation and Forced degradation studies of Bilastine

Asian Journal of Pharmaceutical Analysis ◽

10.52711/2231-5675.2021.00031 ◽

2021 ◽

pp. 183-187

Author(s):

Khushbu K. Patel ◽

Arati M. Patel ◽

C. N. Patel

Keyword(s):

Retention Time ◽

Dosage Form ◽

Method Development ◽

Limit Of Detection ◽

Hplc Method ◽

Forced Degradation ◽

Limit Of Quantification ◽

Pharmaceutical Dosage Form ◽

Ich Guidelines ◽

Hplc Method Development

A new simple, rapid, accurate and precise method for estimation of Bilastine in pharmaceutical dosage form by reverse phase liquid chromatography. The developed method employed mobile phase was Acetonitrile and Ammonium acetate pH 5.0 adjusted with glacial acetic acid with 85:15% v/v and flow rate 1.0ml/min. Method was developed using column C18 Water (150 × 4.6mm, 5µm) and detection wavelength was 215nm. The retention time was found to be 2.519 min. the proposed method was successfully applied to the determination of Bilastine in dosage form. High linearity of developed method was confirmed over concentration range of 25- 150 µg/ml and co-relation co-efficient is 0.996. The percentage RSD for precision and accuracy of the method was found to be less than 2%. The recovery was in the range of 99 – 102% and limit of detection was found to be 0.45µg/ml and limit of quantification was found to be 1.20µg/ml. Bilastine was found to degrade under acid and oxidation conditions. There was no interference of excipient and degradation product in retention time so method was specific. Analytical parameter such as precision, accuracy, limit of detection, limit of quantification and robustness were determined according to international Conference on Harmonization (ICH) guidelines.

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METHOD DEVELOPMENT AND VALIDATION FOR SIMULTANEOUS QUANTIFICATION OF NETUPITANT AND PALONOSETRON IN BULK AND PHARMACEUTICAL DOSAGE FORM AND THEIR FORCED DEGRADATION STUDY BY RP-HPLC

Asian Journal of Pharmaceutical and Clinical Research ◽

10.22159/ajpcr.2019.v12i2.28949 ◽

2019 ◽

pp. 119-123

Author(s):

MANORANJANI M

Keyword(s):

Dosage Form ◽

Method Development ◽

Limit Of Detection ◽

Hplc Method ◽

Forced Degradation ◽

Pharmaceutical Dosage Form ◽

Pharmaceutical Dosage Forms ◽

Degradation Study ◽

Simultaneous Quantification ◽

Relative Standard

Objective: The present paper describes a simple, accurate, and precise reversed-phase high-performance liquid chromatography (HPLC) method for rapid and simultaneous quantification of netupitant (NTP) and palonosetron (PLS) in bulk and pharmaceutical dosage form. Methods: The chromatographic separation was achieved on Luna C18 (250 mm × 4.6 mm, 5 μ). Mobile phase contained a mixture of 0.1% orthophosphoric acid and acetonitrile in the ratio of 60:40 v/v, flow rate 1.0 ml/min, and ultraviolet detection at 222 nm. Results: The proposed method shows a good linearity in the concentration range of 60–900 μg/ml for NTP and 0.1–1.5 μg/ml for PLS under optimized conditions. All the precision and recovery results are in between 98 and 102%. In the entire robustness conditions, percentage of relative standard deviation is <2.0%. Degradation has minimum effect in stress condition and solutions are stable up to 24 h. This method is validated different parameters such as precision, linearity, accuracy, limit of detection, limit of quantification, ruggedness, robustness, and forced degradation study were determined according to the International Conference of Harmonization (ICH) Q2B guidelines. Conclusion: All the parameters of validation were found to be within the acceptance range of ICH guidelines. Since there is no HPLC method reported in the literature for the estimation of NTP and PLS in pharmaceutical dosage forms, there is a need to develop quantitative methods under different conditions to achieve improvement in sensitivity, selectivity, etc. Hence, the author has attempted to develop a validation and forced degradation for simultaneous quantification of NTP and PLS.

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RP-HPLC Method Development and Validation for the Estimation of Sacubitril and Valsartan in Pharmaceutical Dosage Form

Research Journal of Pharmacy and Technology ◽

10.52711/0974-360x.2021.01008 ◽

2021 ◽

pp. 5797-5802

Author(s):

G.M. Kadam ◽

A.L. Puyad ◽

T.M. Kalyankar

Keyword(s):

Dosage Form ◽

Method Development ◽

Limit Of Detection ◽

Hplc Method ◽

Content Uniformity ◽

Phase Detection ◽

Limit Of Quantification ◽

Pharmaceutical Dosage Form ◽

Rp Hplc ◽

Hplc Method Development

A new, economical, simple, accurate, and precise RP-HPLC method was developed for simultaneous assay and content uniformity determination of Sacubitril and Valsartan in bulk and pharmaceutical dosage form. The separation of Sacubitril and Valsartan was achieved within 6 minutes on Phenomenex Luna C18 250 mm x 4.6mm and 5µm Particle Size, column using Acetonitrile: Methanol: Water (30:55:15% v/v/v) as the mobile phase. Detection was carried out at 250 nm wavelength. The retention time of Sacubitril and Valsartan was found to be 2.361 and 3.304 min, respectively. The validation of the developed method was performed in terms of specificity, accuracy, precision, linearity, the limit of detection, the limit of quantification as mentioned in International Conference on Harmonization (ICH) guidelines. The method showed adequate sensitivity concerning linearity, accuracy, and precision over the range 12-36 μg/ml and 13-39 μg/ml for Sacubitril and Valsartan, respectively. The percentage recoveries obtained for Sacubitril and Valsartan were found to be in the range of 98.00 – 102.00 %. The proposed method is suitable for use in quality-control laboratories for quantitative analysis.

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HPLC METHOD DEVELOPMENT FOR ESTIMATION OF RAMELTEON IN TABLET DOSAGE FORM

INDIAN DRUGS ◽

10.53879/id.50.06.p0020 ◽

2013 ◽

Vol 50 (06) ◽

pp. 20-23

Author(s):

S Sahoo ◽

◽

P. K. Panda ◽

S. K. Mishra

Keyword(s):

Flow Rate ◽

Dosage Form ◽

Method Development ◽

Hplc Method ◽

Reverse Phase Hplc ◽

Ich Guidelines ◽

Hplc Method Development ◽

Tablet Dosage ◽

Good Agreement

A simple, fast, accurate and precise reverse phase HPLC method is developed and described for the determination of ramelteon in tablet dosage form. Chromatography was carried on an ODS column using a mixture of acetonitrile and phosphate buffer pH 7.0 (35:65 V/V) as the mobile phase at a flow rate of 1.0 mL/min with detection at 286 nm. The retention time of the drug was 7.7 min. The procedure was validated for linearity, precision, accuracy, and robustness. The developed method was validated for linearity from 50 to 150% which shows the method is quite linear with a correlation coefficient of 0.999, for precision which includes system precision, method precision, intraday and by another analyst on another day, and accuracy. The %RSD for system precision was observed to be 1.1, whereas the method precision was observed to be 0.2. The % recovery from ‘accuracy’ studies yielded the recovery of 99.7-101.5% which indicates the capability of the method, and finally for robustness that includes studies w.r.t. change in flow rate, the percentage of organic modifier and pH. As per ICH guidelines, method validation results are in good agreement. The proposed method was simple, sensitive, precise and accurate.

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NOVEL RP-HPLC METHOD DEVELOPMENT AND VALIDATION FOR ESTIMATION OF TELMISARTAN AND NEBIVOLOL HCL IN PHARMACEUTICAL DOSAGE FORM

Asian Journal of Pharmaceutical and Clinical Research ◽

10.22159/ajpcr.2018.v11i9.27016 ◽

2018 ◽

Vol 11 (9) ◽

pp. 431 ◽

Cited By ~ 1

Author(s):

Heena Ar Shaikh ◽

Vandana Jain

Keyword(s):

High Performance ◽

Dosage Form ◽

Method Development ◽

Limit Of Detection ◽

Hplc Method ◽

Limit Of Quantification ◽

Pharmaceutical Dosage Form ◽

Rp Hplc ◽

Validation Parameters ◽

Hplc Method Development

Objective: A simple, accurate, precise, robust reverse phase high performance liquid chromatography (RP-HPLC) method was developed for the estimation of telmisartan and nebivolol hydrochloride (HCl) simultaneously in its combined dosage form.Methods: The compounds were well resolved in an isocratic method using the mobile phase composition of acetonitrile: Buffer (potassium dihydrogen orthophosphate pH adjusted 3.1 with orthophosphoric acid) in a ratio of 40:60 v/v at a flow rate of 1.2 ml/min using C18 Shim-pack (150 mm × 4.6 mm, 5 μ) column. The detection was carried out at 280 nm.Results: The retention time of telmisartan and nebivolol HCl was 4.8 min and 6.5 min, respectively. The developed method was validated by evaluating various validation parameters such as linearity, precision, accuracy, robustness, specificity, limit of detection, and limit of quantification according to the international council for harmonization guidelines. The standard calibration curve was obtained in the concentration range of 24–56 μg/ml for telmisartan and 3–7 μg/ml for nebivolol HCl. The overall average % recovery was found out to be 100.35 for telmisartan and 98.84 for nebivolol HCl.Conclusion: Statistical analysis of the data showed that the method is reproducible and selective for the estimation of telmisartan and nebivolol HCl. The proposed method could be used for analysis of telmisartan and nebivolol HCl in their dosage form.

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