Development and Validation of Stability Indicating High-Performance Liquid Chromatographic Method for Determination of Cyproheptadine Hydrochloride, its Impurity And Degradation Product

2020 ◽  
Author(s):  
Maha M Abdelrahman ◽  
Eglal A Abdelaleem ◽  
Nouruddin W Ali ◽  
Raghda A Emam
Keyword(s):  
Degradation Product ◽  
High Performance ◽  
Oxidative Degradation ◽  
High Performance Liquid Chromatographic ◽  
Hplc Method ◽  
Pharmaceutical Formulation ◽  
Good Resolution ◽  
Intermediate Precision ◽  
Rp Hplc

Abstract This work presents a sensitive, accurate and selective RP-HPLC method for simultaneous determination of cyproheptadine HCl (CPH), its impurity B (dibenzosuberone) and CPH oxidative degradation product (10,11-dihydroxy-dibenzosuberone) in bulk powder and in pharmaceutical formulation. The RP-HPLC method depends on isocratic elution using C8 column and mobile phase consisting of 0.05 M KH2PO4 buffer:methanol (35:65, v/v, pH = 4.5) at a flow rate of 2 mL/min, and the eluant was monitored at 245 nm. Good resolution was obtained with tR values of 3.05, 7.54 and 6.17 min for CPH, impurity and oxidative degradate, respectively. The proposed method has been validated as per ICH guidelines using pure forms of CPH, its impurity and degradation product in pharmaceutical formulation with an accuracy of 100.48, 100.16 and 100.11, respectively. Additional spiking experiments yielded an accuracy of 100 ± 1.6%. Repeatability and intermediate precision results indicated acceptable low <2% RSD values. Moreover, the developed method’s statistical results were favorably compared to the previously reported method results regarding both accuracy and precision. The developed method can be applied for analysis of the three components in quality control laboratories.

scholarly journals ANALYTICAL METHOD DEVELOPMENT AND VALIDATION OF ATOMOXETINE HYDROCHLORIDE USING RAPID HIGH-PERFORMANCE LIQUID CHROMATOGRAPHIC TECHNIQUE

2018 ◽  
Vol 11 (11) ◽  
pp. 118
Author(s):  
Zubaidur Rahman ◽  
Vijey Aanandhi M ◽  
Sumithra M
Keyword(s):  
High Performance ◽  
Method Development ◽  
High Sensitivity ◽  
High Performance Liquid Chromatographic ◽  
Hplc Method ◽  
Chromatographic Technique ◽  
Pharmaceutical Dosage Form ◽  
Rp Hplc ◽  
Liquid Chromatographic

Objective: A simple, novel, sensitive, rapid high-performance liquid chromatographic (RP-HPLC) method has been developed and validated for quantitative determination of atomoxetine HCl (ATH) in bulk and formulations.Methods: The chromatographic development was carried out on RP-HPLC. The column used as Xterra RP 18 (250 mm × 4.6 mm, 5 μ particle size), with mobile phase consisting of methanol: water 80:20 V/V. The flow rate was 1.0 mL/min and the effluents were monitored at 270 nm.Results: The retention time was found to be 5.350 min. The method was validated as per International Conference on Harmonization Guideline with respect to linearity, accuracy, precision, and robustness. The calibration curve was found to be linear over a range of 2–10 μg/mL with a regression coefficient of 0.9999. The method has proved high sensitivity and specificity.Conclusion: The results of the study showed that the proposed RP-HPLC method was simple, rapid, precise and accurate which is useful for the routine determination of ATH in bulk drug and in its pharmaceutical dosage form.

scholarly journals ESTIMATION OF AMLODIPINE BESYLATE AND IRBESARTAN IN PHARMACEUTICAL FORMULATION BY RP-HPLC WITH FORCED DEGRADATION STUDIES

2019 ◽  
pp. 159-167 ◽  
Author(s):  
T Hemant Kumar ◽  
CH. ASHA ◽  
D. GOWRI SANKAR
Keyword(s):  
High Performance ◽  
High Performance Liquid Chromatographic ◽  
Hplc Method ◽  
Pharmaceutical Formulation ◽  
Forced Degradation ◽  
Amlodipine Besylate ◽  
Reverse Phase ◽  
Rp Hplc ◽  
Forced Degradation Studies ◽  
Liquid Chromatographic

Objective: To develop and validate a simple, specific, accurate, precise and sensitive reverse phase high performance liquid chromatographic (RP-HPLC) method with forced degradation studies for the simultaneous estimation of amlodipine besylate and irbesartan in the pharmaceutical formulation. Methods: The chromatographic separation of the two drugs were achieved using Enable C 18G column (250 ×4.6 mm; 5 µm) in isocratic mode with mobile phase consisting of sodium acetate buffer (pH 4.0) and acetonitrile (30:70, % v/v) with a flow rate of 0.6 ml/min. Ultraviolet(UV) detection was carried out at 238 nm. The proposed method was validated for linearity, range, accuracy, precision, robustness, limit of detection (LOD) and limit of quantification (LOQ). The tablet formulation was subjected to stress conditions of degradation including acidic, alkaline, oxidative, thermal and photolysis. Results: The retention time for amlodipine besylate and irbesartan were found to be 5.512 and 6.321 min respectively. Linearity was observed over a concentration range 4-32 µg/ml for amlodipine besylate (r2 =0.9999) and 10-70 µg/ml for Irbesartan (r2 =0.9998). The % relative standard deviation (RSD) for Intraday and Interday precision was found to be 0.436 and 0.699 for amlodipine besylate and 0.435 and 0.30 for irbesartan. Amlodipine besylate shown stability towards acidic and thermal whereas in basic, oxidative and photolytic it shown less stability in which it degraded to more extent. Irbesartan shown stability towards thermal conditions whereas in remaining conditions it degrades to more extent especially in oxidative conditions. Conclusion: The developed reverse phase high performance liquid chromatographic (RP-HPLC) method was also found to be simple, precise and sensitive for the simultaneous determination of amlodipine besylate and irbesartan in the tablet dosage form.

scholarly journals Stability-Indicating Method for Determination of Oxyphenonium Bromide and Its Degradation Product by High-Performance Liquid Chromatography

2007 ◽  
Vol 90 (5) ◽  
pp. 1250-1257 ◽  
Author(s):  
Alaa EL-Gindy ◽  
Samy Emara ◽  
Heba Shaaban
Keyword(s):  
Degradation Product ◽  
High Performance ◽  
Potassium Dihydrogen Phosphate ◽  
Order Rate Constant ◽  
High Performance Liquid Chromatographic ◽  
Hplc Method ◽  
Dihydrogen Phosphate ◽  
Stability Indicating Method ◽  
Oxyphenonium Bromide

Abstract A high-performance liquid chromatographic (HPLC) method was developed for determination of oxyphenonium bromide (OX) and its degradation product. The method was based on the HPLC separation of OX from its degradation product, using a cyanopropyl column at ambient temperature with mobile phase of acetonitrile25 mM potassium dihydrogen phosphate, pH 3.4 (50 + 50, v/v). UV detection at 222 nm was used for quantitation based on peak area. The method was applied to the determination of OX and its degradation product in tablets. The proposed method was also used to investigate the kinetics of the acidic and alkaline degradation of OX at different temperatures, and the apparent pseudo first-order rate constant, half-life, and activation energy were calculated. The pH-rate profile of the degradation of OX in Britton-Robinson buffer solutions within the pH range 212 was studied.

A HPLC-UV Method for Simultaneous Determination of Hypocrellin A and B from Fermentation Broth of Shiraia Bambusicola LPHP-89

2015 ◽  
Vol 1092-1093 ◽  
pp. 662-665
Author(s):  
Sai Dan Zhang ◽  
Ping Lv ◽  
Xiu Zhu
Keyword(s):  
High Performance ◽  
Fermentation Broth ◽  
High Performance Liquid Chromatographic ◽  
Hplc Method ◽  
Shiraia Bambusicola ◽  
Rp Hplc ◽  
Hypocrellin A ◽  
Hypocrellin B ◽  
Liquid Chromatographic

A rapid, sensitive and reproducible high performance liquid chromatographic (HPLC) method was developed and validated for simultaneous quantification of hypocrellin A, hypocrellin B from Fermentation Broth of Shiraia bambusicola LPHP-89. Isocratic RP-HPLC system with C18 column (4.6 mm × 250 mm i.d., 5 μ particle size) and a detector UV-VWD was employed. The mobile phase consisted of methanol、water and acetic acid (60:40:1, v/v/v) and was pumped at a flow rate of 1.0 mL/min. The injection volume was5 μL. The quantitation wavelength was set at 254 nm.Total run time was 20 min and retention times for hypocrellin A and hypocrellin B were 10.06 and 15.38 min, respectively.

scholarly journals Development and Validation of Estimation of Genotoxic Impurity (Hydroxylamine Hydrochloride content) in Leflunomide by using RP-HPLC technique

2021 ◽  
Vol 37 (02) ◽  
pp. 493-498
Author(s):  
Mohan Bhatale ◽  
Neelakandan Kaliyaperumal ◽  
Gopalakrishnan Mannathusamy ◽  
Gurunathan Ramalingam
Keyword(s):  
Mobile Phase ◽  
High Performance ◽  
Hydroxylamine Hydrochloride ◽  
High Performance Liquid Chromatographic ◽  
Hplc Method ◽  
Intermediate Precision ◽  
Rp Hplc ◽  
System Suitability ◽  
Development And Validation ◽  
Liquid Chromatographic

A simple, selective, linear having accuracy and specific of reverse phase high-performance liquid chromatographic (RP-HPLC) method for determination of Genotoxic impurity Hydroxylamine Hydrochloride of drug Leflunomide is reported.The separation and analysis were done on YMC Triart C18 (4.6 mm x 150 mm), having particle size 3.0 μm. KH2PO4 in 2000 mL of purified water and 2 mL triethylamine with pH 2.5 with phosphoric acid is mobile phase-A while acetonitrile is mobile Phase-B with gradient program. The elution achieved with 1.50 mL/min flow rate and using UV detection at 230 nm wavelength. Selected column oven temperature is 45°C and auto sampler 5°C respectively. In this method linearity and accuracy of Hydroxylamine HCl covered with specification limit of LOQ to 150 % (i.e.3 to 23 ppm). The observed correlation coefficient is 0.99965 and recovery in between 99.07 to 114.94. In method precision (ie.repeatability) and intermediate precision (IP) observed % RSD of six spiked test preparation is below 5.0 %. The standard and sample were stable for 3 days when stored at 2 to 8°C temperature. In robustness studies system suitability parameters ie tailing factor, theoretical plates and %RSD does not show significant changes. The present RP-HPLC method is selective, robust, linear, and precise for detection of Hydroxylamine HCl.

scholarly journals RP-HPLC method development and validation for simultaneous estimation of Cilnidipine, Atenolol and Chlorthalidone

2018 ◽  
Vol 8 (6-s) ◽  
pp. 78-82 ◽  
Author(s):  
Vishal Singh Solanki ◽  
RAM SINGH BISHNOI ◽  
Raviraj Baghel ◽  
Deepti Jain
Keyword(s):  
High Performance ◽  
Chromatographic Method ◽  
Method Development ◽  
High Performance Liquid Chromatographic ◽  
Hplc Method ◽  
Simultaneous Estimation ◽  
Good Resolution ◽  
Rp Hplc ◽  
Tablet Dosage ◽  
Liquid Chromatographic

A simple precise and economical reverse phase high performance liquid chromatographic method has been developed and validated for the simultaneous estimation of Cilnidipine (CDP), Atenolol (ATL) and Chlorthalidone (CTD).The chromatographic separation was achieved by using Hypersil- keystone C18 (4.6 x 250mm, 5μm) under isocratic conditions The mobile phase consisted of methanol and triple distilled water (80/20, v/v) having pH 7 with a flow rate of 1.0 mL/min. The eluents were monitored at 225 nm for simultaneous measurement.The selected chromatographic conditions were found to effectively separate CDP (Rt: 3.25 min), ATL (Rt: 5.366 min) and CTD (Rt: 9.025 min) having good resolution. The developed method was validated for linearity, accuracy, precision, LOD, LOQ, robustness and for system suitability parameters as per ICH guidelines. In this study, an excellent linearity was obtained with r2 = 0.999, r² = 0.999, r² = 1, for CDP, ATL and CTD respectively. The developed chromatographic method proved to be simple, precise, accurate, robust and reproducible Thus, this method would be employed for routine simultaneous quantification of CDP, ATL and CTD in bulk form or tablet dosage form.   Keywords: Cilnidipine, Atenolol and Chlorthalidone, RP-HPLC.

scholarly journals HPLC METHOD FOR SIMULTANEOUS DETERMINATION OF METFORMIN AND SITAGLIPTIN IN PHARMACEUTICAL DOSAGE FORMS AND ITS APPLICATIONS TO DISSOLUTION STUDY

2019 ◽  
Vol 3 (7) ◽  
Author(s):  
Hemraj Sharma ◽  
Boya Madhuri ◽  
Yiragamreddy Padmanabha Reddy ◽  
Kondareddy Vinod Kumar ◽  
Nanda Kishor Bhatta ◽  
...  
Keyword(s):  
Simultaneous Determination ◽  
High Performance ◽  
High Performance Liquid Chromatographic ◽  
Dosage Forms ◽  
Hplc Method ◽  
Uv Detector ◽  
Pharmaceutical Dosage Forms ◽  
Dissolution Study ◽  
Rp Hplc

A novel approach was used to develop and validate a rapid, specific, accurate and precise Reverse phase High performance liquid chromatographic (RP-HPLC) method for the simultaneous determination of Metformin and Sitagliptin in pharmaceutical dosage forms and its applications to dissolution study. The chromatographic separation was carried out on a C8 (250mm X 4.6 mm i.d., 5μm) column with a mobile phase of 40 Acetonitrile: 60 Phosphate Buffer (pH 6.8), using UV detector at 257 nm at 1ml min-1 flow rate. The retention time for Metformin was 2.11 minutes and 5.30 minutes for Sitagliptin. The Linearity for Metformin was found to be 10-80 µg ml-1 with R2 value of 0.9998 and for Sitagliptin 1-8 µg ml-1 with R2 value of 0.9976. Dissolution study of both for Metformin and Sitagliptin was carried, Percentage of drug release was established which was found to be 96.23% and 102.64% respectively, in the period of 50 minutes. Keywords: RP-HPLC, Metformin, Sitagliptin, Dissolution study

scholarly journals Development and validation for determination of lisinopril dihydrate in bulk drug and formulation using RP-HPLC method

2018 ◽  
Vol 3 (2) ◽  
pp. 14-18
Author(s):  
Zahid Zaheer ◽  
Sarfaraz Khan ◽  
Mohammad Sadeque ◽  
Hundekari G. I. ◽  
Rana Zainuddin
Keyword(s):  
High Performance ◽  
High Performance Liquid Chromatographic ◽  
Hplc Method ◽  
Rp Hplc ◽  
Liquid Chromatographic Method ◽  
Bulk Drug ◽  
Development And Validation ◽  
Liquid Chromatographic ◽  
Isocratic Mode

A simple, reproducible and efficient reverse phase high performance liquid chromatographic method was developed for Lisinopril in bulk drug and formulation. A column having 150 × 4.6 mm in isocratic mode with mobile phase containing acetonitrile: phosphate buffer (70:30; adjusted to pH 3.0) was used. The flow rate was 0.8 ml/min and effluent was monitored at 216 nm. The retention time (min) and linearity range (μg/ml) for Lisinopril was (1.510) and (10-35). The developed method was found to be accurate, precise and selective for determination of Lisinopril in bulk and formulation.

scholarly journals Validated RP-HPLC Method for the Determination of Ivabradine Hydrochloride in Pharmaceutical Formulation

2017 ◽  
Vol 9 (05) ◽  
Author(s):  
MD. Muzaffar -ur- Rehman1 ◽  
G. Nagamallika
Keyword(s):  
Mobile Phase ◽  
Dosage Forms ◽  
Hplc Method ◽  
Pharmaceutical Formulation ◽  
Intermediate Precision ◽  
Pharmaceutical Dosage Forms ◽  
Rp Hplc ◽  
Ich Guidelines ◽  
Bulk Drug

A simple, rapid, precise, and accurate RP-HPLC method for the estimation of Ivabradine Hydrochloride an anti-anginal agent, both as a bulk drug and in pharmaceutical formulation was developed. The chromatographic separation was achieved on a Thermosil C18 150 × 4.5 mm, 5μm column by using a mobile phase containing a mixture of methanol and phosphate buffer pH 6.5 in the ratio of 65:35 % v/v at a flow rate of 1ml/min and at an ambient temperature. The detection was monitored at a wavelength of 265nm. A clear chromatographic peak was identified with the retention time of 4.36 min and tailing factor of 1.23. The developed method was validated according to ICH guidelines with respect to specificity, linearity, accuracy, precision and robustness. The method shows a good linear relationship with correlation co-efficient of more than 0.992 in the concentration range of 30μg-150μg. The method showed mean % Recovery of 100.4% and %RSD for repeatability and intermediate precision was less than 2%. The proposed method can be used successfully for the quantitative determination of Ivabradine HCL in pharmaceutical dosage forms.

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