scholarly journals Development and Validation of Estimation of Genotoxic Impurity (Benzimidamidecontent) in Leflunomide by Using RP-HPLC Technique

2021 ◽  
pp. 78-85
Author(s):  
Mohan Bhatale ◽  
Neelakandan Kaliyaperumal ◽  
Gopalakrishnan Mannathusamy ◽  
Gurunathan Ramalingam
Keyword(s):  
High Performance ◽  
Room Temperature ◽  
High Performance Liquid Chromatographic ◽  
Hplc Method ◽  
Reverse Phase ◽  
Intermediate Precision ◽  
Rp Hplc ◽  
Development And Validation ◽  
Liquid Chromatographic ◽  
Program Mode

The measurement of Genotoxic contaminant, a simple, selective, linear, accurate, and specific reverse phase high-performance liquid chromatographic (RP-HPLC) process was proposed. A Benzimidamide impurity in the medication Leflunomide has been discovered. Separation and analysis were carried out on Zorbax SB phenyl (4.6 mm x 250 mm) with a particle size of 5.0 μm. with 0.1 % Triethylamine in purified water with a pH of 7.0 and a buffer of phosphoric acid (20% in water). The mobile phase is a 40:60 mixture of buffer and Acetonitrile with degassing. Isocratic program mode was used. The elution was carried out at a rate of 1.0 mL/min with UV detection at a wavelength of 289 nm. The temperature of the selected column oven is 25°C. The linearity and accuracy of Benzimidamide are covered in this approach, with a LOQ limit of 150 percent (i.e.0.03 to 0.45 ppm). The observed correlation coefficient is 0.99994, with a range of 100.01 to 104.8 for recovery. The measured percent RSD of six spiked test preparation is below 5.0 percent in procedure precision (i.e. repeatability) and intermediate precision (IP). When maintained at room temperature, the standard and sample remained stable for three days. System appropriateness characteristics such as tailing factor and percent RSD do not exhibit significant changes in robustness experiments. For the detection of Benzimidamide the present RP-HPLC method is act as selective, robust, linear and precise.

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

2021 ◽  
Vol 37 (2) ◽  
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.

Development and Validation of RP-HPLC method for the Estimation of Ritonavir in API and tablet Formulation

2021 ◽  
pp. 5457-5460
Author(s):  
Avinash Birajdar ◽  
Varsha Tegeli ◽  
Suyash Ingale ◽  
Gajanand Nangare
Keyword(s):  
High Performance ◽  
Pharmaceutical Formulations ◽  
High Performance Liquid Chromatographic ◽  
Hplc Method ◽  
Tablet Formulation ◽  
Reverse Phase ◽  
Rp Hplc ◽  
Liquid Chromatographic Method ◽  
Development And Validation ◽  
Liquid Chromatographic

A Reverse Phase High Performance Liquid Chromatographic method has been developed and validated for estimation of Ritonavir in API and Tablet formulation. The chromatographic separation was carried out using ZOROBAX Bonus-RP C-18 column (250 x 4.6mm, 5µm) as stationary phase and Methanol: Acetonitrile: 0.1% Trifluoroacetic acid water (81:9:10) as mobile phase at 1.0 ml/min flow rate and detection was carried out at 250 nm. The method was validated accordance to the Guidelines of International Council for Harmonization (ICH). Ritonavir have linearity in the concentration range of 50-150µg/ml with correlation coefficient (r2=1) respectively. Ritonavir eluted at 3.05 min respectively. The method is sensitive, precise and accurate. So, the method can be successfully applied for the routine analysis of Ritonavir in pharmaceutical formulations.

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 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.

Development and Validation of RP-HPLC Method for Simultaneous Estimation of Gatifloxacin and flurbiprofen Sodium in Eye Drops

2019 ◽  
Vol 9 (01) ◽  
pp. 83-88
Author(s):  
Pinkal Patel ◽  
Nalini Patel ◽  
Kinjal Parmar
Keyword(s):  
High Performance ◽  
Pharmaceutical Formulations ◽  
High Performance Liquid Chromatographic ◽  
Reversed Phase ◽  
Hplc Method ◽  
Simultaneous Estimation ◽  
Eye Drops ◽  
Rp Hplc ◽  
Development And Validation ◽  
Liquid Chromatographic

A simple, selective and rapid reversed phase High Performance Liquid Chromatographic (RP-HPLC) method has been developed and validated for the simultaneous analysis Gatifloxacin and flurbiprofen sodium in eye drops. The separation was carried out using a mobile phase consisting ACN: Buffer (pH 3.5) in the ratio of 55:45 v/v. The column used was Phenomenex luna ODS C18 (250mm X 4.6 mm i.d., 5 μm particle size) with flow rate of 1 ml / min using UV detection at 268 nm. The described method was linear over a concentration range of 2-12 μg/ml for both of Gatifloxacin and flurbiprofen sodium. The retention times of Gatifloxacin and flurbiprofen sodium were found to be 3.710 min. and 6.797 min respectively. Method was validated statistically and recovery studies were carried out. The proposed method has been applied successfully to the analysis of cited drugs either in pure form or in pharmaceutical formulations with good accuracy and precision. The method here in described can be employed for quality control and routine analysis of drugs in pharmaceutical formulations.

DEVELOPMENT AND VALIDATION OF RP-HPLC METHOD FOR THE ESTIMATION OFTRANDOLAPRIL AND VERAPAMIL IN COMBINED TABLET DOSAGE FORM

INDIAN DRUGS ◽  
2012 ◽  
Vol 49 (05) ◽  
pp. 61-64
Author(s):  
A. L Rao ◽  
◽  
R. V Bhaskara
Keyword(s):  
High Performance ◽  
Dosage Form ◽  
High Performance Liquid Chromatographic ◽  
Hplc Method ◽  
Rp Hplc ◽  
Ich Guidelines ◽  
Liquid Chromatographic Method ◽  
Development And Validation ◽  
Tablet Dosage ◽  
Liquid Chromatographic

A reverse phase high performance liquid chromatographic method was developed and validated asper ICH guidelines for estimation of trandolapril and verapamil in combined tablet dosage form. Theseparation was obtained using a mobile phase consisting of acetonitrile and phosphate buffer adjustingpH to 3.0 in the ratio of 70:30 v/v and using Waters C18 (250 x 4.6 mm, 5 mcm) column maintained atambient temperature. The flow rate was 1.2 mL min-1 and UV detection was monitored at 215 nm. Theretention time (min) and linearity range (mcg mL-1) for trandolapril and verapamil were (5.12, 2.70) and(20-60, 20-60), respectively. The method validation results are within the acceptance criteria for precision,accuracy and linearity. The proposed method was found to be suitable for routine quality control ofmarketed formulation containing these APIs.

scholarly journals METHOD DEVELOPMENT AND VALIDATION FOR ESTIMATION OF CURCUMIN AND PIPERINE BY RP-HPLC

2019 ◽  
Vol 11 (1) ◽  
pp. 216 ◽  
Author(s):  
Ramya Kuber B.
Keyword(s):  
High Performance ◽  
Method Development ◽  
Limit Of Detection ◽  
High Performance Liquid Chromatographic ◽  
Hplc Method ◽  
Reverse Phase ◽  
Limit Of Quantification ◽  
Average Percentage ◽  
Rp Hplc ◽  
Liquid Chromatographic

Objective: To develop a simple, sensitive, specific, accurate reverse phase high performance liquid chromatographic (RP-HPLC) method for the estimation of curcumin and piperine.Methods: The separation was done using a column Inertsil–ODS C18 (250 mm × 4.6 mm, 5µ particle size) and mobile phase composed of methanol: water (45:55 v/v), flow rate at 1 ml/min and detection was carried out at 282 nm with photodiode array (PDA) detector.Results: The separation of curcumin and piperine were found to be at the retention time of 2.433 min and 3.095 min, respectively. The method was found to be linear at a concentration range 20-80 µg/ml for curcumin and piperine. The limit of detection (LOD) and limit of quantification (LOQ) was found to be 0.05µg/ml and 0.17µg/ml for curcumin and 0.18µg/ml and 0.53µg/ml for piperine respectively. The average percentage recoveries of curcumin and piperine were in the range of 98-100.6%.Conclusion: A simple and sensitive reverse phase high performance liquid chromatographic method was developed for the estimation of curcumin and piperine.

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