Analytical Method Development and Validation of Etravirine by RP-UFLC

2021 ◽  
pp. 3537-3542
Author(s):  
Barath M ◽  
Chandan R. S ◽  
Maruthi R ◽  
Paramakrishnan N
Keyword(s):  
Mobile Phase ◽  
Method Development ◽  
Detection System ◽  
Persistence Time ◽  
Ich Guidelines ◽  
Method Development And Validation ◽  
Fast Liquid Chromatography ◽  
Reliability And Robustness ◽  
Development And Validation ◽  
Alkaline Corrosion

An ultra-fast liquid chromatography (RP-UFLC) approach was processed for the estimation of ETR, which is quick, responsive, reliable, and inexpensive. Work on the Phenomenex Kinetex C18 column (250x 4,6mm. 5μ) was carried out with MeOH and acetonitrile in the mobile phase ratio of (60:40v/v) at 1.0mL/min. With a PDA detection system, the eluent was tracked at 311nm. ETR elutes at a persistence time of 3.226 min. The proposed method gives linearity of concentration from 1 to 5μg/mL, with the value of R2 at 0.9942%. For the proposed method, LOD and LOQ are measured as 0.02 and 0.073μg/mL. The pharmaceutical drug included acidic, alkaline, corrosion, Ultraviolet, and heat stress stipulations. The deterioration material was nicely resolved from ETR peaks, which showed the reliability of the process. The approach has been tested with respect to process adequacy, linearity, reliability, and robustness, as per ICH guidelines.

scholarly journals Method Development and Validation of RP-HPLC Method for the Estimation of Ormeloxifene

2017 ◽  
Vol 2 (03) ◽  
pp. 78-82
Author(s):  
Anusha Shivaraj ◽  
Shireesha Battula
Keyword(s):  
Mobile Phase ◽  
Room Temperature ◽  
Method Development ◽  
Hplc Method ◽  
Rp Hplc ◽  
Ich Guidelines ◽  
Method Development And Validation ◽  
Development And Validation ◽  
Isocratic Mode ◽  
Ich Guideline

A new simple, specific, accurate, precise RP-HPLC method has been developed for the estimation of Ormeloxifene. The chromatographic separation for Ormeloxifene was achieved with mobile phase containing methanol :ACN(70:30 v/v), agilent C18 column (4.6 x150 mm) 5 μ at room temperature and UV detection at 274nm.The compounds were eluted in the isocratic mode at a flow rate of 1ml/min. The retention time of Ormeloxifene was found to be 2.497min. The method was validated according to ICH guideline for linearity, specificity, precision, accuracy, LOD, LOQ and robustness in accordance with ICH guidelines.

scholarly journals Analytical method development and validation of assay test of pravastatin sodium tablets

2019 ◽  
Vol 9 (2) ◽  
pp. 70-75
Author(s):  
Ashvini C Shinde ◽  
Nitin V Devhadrao ◽  
Ashwini S Bansode ◽  
Ajit S Bansode
Keyword(s):  
Mobile Phase ◽  
Method Development ◽  
Solution Stability ◽  
Pravastatin Sodium ◽  
Ich Guidelines ◽  
Method Development And Validation ◽  
Acquity Uplc ◽  
Development And Validation ◽  
Tablet Dosage ◽  
Liquid Chromatographic

A simple, accurate, precise and stability indicating Ultra performance liquid chromatographic method for determination of pravastatin sodium in tablet dosage form. The separation was carried on Acquity UPLC ® HSS C18, 2.1 × 100mm, 1.8µm ID column, with mobile phase comprising of mixture of pH 5.5 buffer: methanol in the ratio of 30 : 70 v/v, as the mobile phase at a flow rate  0.2 ml/min and the detection was carried out using UV-visible detector at 238nm. The method was validated by evaluation of different parameters such as accuracy, precision, linearity, ruggedness, robustness, filter equivalency, solution stability. The retention time were found to be 1.5 min. Calibration curves were linear with correlation coefficient (r2) 0.999. The Percent assay of Pravastatin sodium tablet was found to be 98.4%. The developed methods were validated as per the ICH guidelines. Keywords: Pravastatin sodium (PVS), UPLC, Method Validation.

scholarly journals Bioanalytical method development and validation for the determination of metoprolol and meldonium in human plasma

Pharmacia ◽  
2020 ◽  
Vol 67 (2) ◽  
pp. 39-48
Author(s):  
Mariana Horyn ◽  
Liliya Logoyda
Keyword(s):  
Formic Acid ◽  
Human Plasma ◽  
Mobile Phase ◽  
Method Development ◽  
Accurate Method ◽  
Ich Guidelines ◽  
Method Development And Validation ◽  
Phase Water ◽  
Development And Validation

Aim.The main purpose of this study was to develop a simple, precise, rapid and accurate method for the quantification of metoprolol and meldonium in human plasma. Materials and methods. The resolution of peaks of metoprolol was best achieved with Discovery C18, 50 × 2.1 mm, 5 μm column and meldonium - ZORBAX HILIC Plus, 50 × 2.1 mm, 3.5 μm column. Samples of metoprolol were chromatographed in a gradient mode (eluent A (acetonitrile – water – formic acid, 5 : 95 : 0.1 v/v), eluent B (acetonitrile – formic acid, 100 : 0.1 v/v)). The initial content of the eluent B is 0%, which increases linearly by 1.0 min to 100% and to 1.11 min returns to the initial 0%. The mobile phase was delivered at a flow rate of 0.400 mL/min into the mass spectrometer ESI chamber. The injection volume was 5μl. Samples of meldonium were chromatographed in a isocratic using mobile phase water – acetonitrile – ammonium formate buffer 200 мМ, 20 : 75 : 5 v/v). Results.The total chromatographic run time was 2.0 minutes and the elution of metoprolol, meldonium and IS occurred at ~1.39 and 1.18 minutes, respectively.A linear response function was established at 2 - 200 ng/mL for metoprolol and 50 -5000 ng/mL for meldonium in human plasma. The% mean recovery for metoprolol in LQC, MQC and HQC was 99.0%, 107.5% and 96.8%, for meldonium in LQC, MQC and HQC was 94.1%, 100.2% and 93.1% respectively. The lowest concentration with the RSD <20% was taken as LLOQ and was found to be 2.31 ng/mL for metoprolol, 47.70 ng/mL for meldonium. The % accuracy of LLOQ samples prepared with the different biological matrix lots were found 115.4% for metoprolol and 95.5% for meldonium, which were found within the range of 80.00–120.00% for the seven different plasma lots. % CV for LLOQ samples was observed as 12.8% and 7.7% respectively, which are within 20.00% of the acceptance criteria. Conclusion.A rapid method was developed for simultaneous determination of metoprolol and meldonium in human plasma. The method was strictly validated according to the ICH guidelines. Acquired results demonstrate that proposed strategy can be effortlessly and advantageously applied for routine examination of metoprolol and meldonium in human plasma.

High Performance HPLC-UV Method Development and Validation for Sulfadoxine from its Potential Interfering Impurities

2021 ◽  
Vol 08 ◽  
Author(s):  
Nayan S. Gadhari ◽  
Jayram V. Gholave ◽  
Suyog S. Patil ◽  
Ajay R. Patil ◽  
Kiran F. Shelke ◽  
...  
Keyword(s):  
Mobile Phase ◽  
High Performance ◽  
Method Development ◽  
Degradation Products ◽  
Drug Product ◽  
Ich Guidelines ◽  
Daunting Task ◽  
Method Development And Validation ◽  
The Stability ◽  
Development And Validation

Objective: To address the separation of interfering potential impurities associated with the drug is always a daunting task. We present the method validation and quantitative determination of sulfadoxine (SUL), an anti-malarial drug with most important interfering impurities present pharmaceutical dosages and in bulk samples using HPLC-UV method. Methods: The UV detection was obtained at 270 nm and SUL is separated on Sunfire C18 (25 cm x 4.6 mm x 5 µ m) column at 45°C with flow rate of 1.0 mL/min in a mobile phase (CH3COOH:CH3CN). The stress testing (acidic/basic/oxidative) was performed using HPLC for SUL and its impurities showing the highly efficient separation peaks between degradant and drug product. Results: The developed method was found to be highly accurate and sensitive in regulation with ICH guidelines. Also, it was found to be free from interference from degradation products which allows the stability indicating capability of developed HPLC-UV method for SUL for validation in bulk drugs. Conclusion: The main advantages of the present method; (a) Separation achieved in 30 minutes, (b) MS compatible mobile phase renders this developed method can be directly adapted to LC-MS without any major modifications in near future, and (c) separation of twelve impurities on Sunfire C18 column. The CFs (correction factors) had been calculated for all the impurities. It was found to be 1.6 (IMP IX), 1.70 (IMP XI) and in between 0.8-1.3 for all other impurities. The LOD of the developed method for all the analytes were in the range of 0.05 to 0.11 μg/mL and the LOQ values were in the range of 0.17 to 0.36 μg/mL.

scholarly journals A New Quantitative Analytical Method Development and Validation for the Analysis of Boceprevir in Bulk and Marketed Formulation

2018 ◽  
Vol 10 (03) ◽  
Author(s):  
Bhetanabotla Chandramowli ◽  
B.M Syam Kumar ◽  
D.V. R. N. Bhikshapathi ◽  
Bigala B Rajkamal
Keyword(s):  
Chromatographic Analysis ◽  
Mobile Phase ◽  
Method Development ◽  
Hplc Method ◽  
Capsule Formulation ◽  
Rp Hplc ◽  
Ich Guidelines ◽  
Validation Parameters ◽  
Method Development And Validation ◽  
Development And Validation

A simple, precise and accurate RP-HPLC technique was developed and the developed method was validated for the regular analysis of Boceprevir. Chromatographic analysis was performed by selecting X-Terra ODS ( C18) column (4.6 mm i.d. × 250 mm, 5μ), Acetonitrile : Phosphate buffer pH -3 ( 90 : 10% v/v) as mobile phase, 1.0 ml/min as flow rate and 20μl injection volume. The LC chromatographic peak was eluted at 3.6 min at 235 nm as UV detection wavelength. The developed method was validated as per the ICH guidelines and the Validation parameters were specificity, accuracy, linearity, precision, LOD and LOQ. Linear relationship for Boceprevir established in the concentration range of 50 to 150μg/mL. Accuracy in terms of percentage recovery found in the range between 98 to 101%. LOD and LOQ values were found to be 2.3 and 7.123μg/mL respectively. The results of the method established that the new RP-HPLC method is convenient and simple in regular analysis of Boceprevir in bulk and capsule formulation.

scholarly journals Method Development and Validation of Salmeterol xinofoate by HPLC

2021 ◽  
Vol 6 (6) ◽  
pp. 52-63
Author(s):  
Sahebrao H. Shembade ◽  
Sagar S. Landage ◽  
Ashapak M. Tamboli ◽  
Ritesh S. Bhate ◽  
Kaustubh V. Gavali ◽  
...  
Keyword(s):  
Mobile Phase ◽  
High Performance ◽  
Method Development ◽  
Quantitative Estimation ◽  
Hplc Method ◽  
Chromatography Method ◽  
Ich Guidelines ◽  
Method Development And Validation ◽  
Liquid Chromatography Method ◽  
Development And Validation

A rapid and precise high performance liquid chromatography method has been developed for the validation of Salmeterol xinofoate in its pure dosage form. The separation was carried out on Agilent Zorbax Bonus RP- (250mm ×4.6mm 5μ) column with a mobile phase consisting of 0.1% Formic acid: Acetonitrile in the ratio of 64:36 v/v as a mobile phase and flow rate is 1ml/min. The detection was carried out at wavelength 234nm. The column thermostatically controlled at 30℃. The retention time of Salmeterol was found to be 1.96 min. The Salmeterol xinofoate followed linearity in the concentration range of 40-60μg/mL with r2= 0.999. The developed method was validated for sensitivity, accuracy and precision. The sample was scanned from 200- 400nm with PDA detector. The % recovery of sample was found to be. The LOD and LOQ of the Salmeterol xinofoate was found to be 2.67μg/ml and 8.08μg/ml respectively. The suitability of this HPLC method for quantitative estimation of Salmeterol xinofoate was proved by validation by the requirements of ICH guidelines.

Method Development and Validation for Estimation of related Substances in Tilorone Dihydrochloride using RP¬-HPLC

2021 ◽  
pp. 3319-3324
Author(s):  
M. Zeba Baktiyar ◽  
B. Mohammed Ishaq ◽  
Siva Sanker Reddy L ◽  
Sreenivasulu M.
Keyword(s):  
Mobile Phase ◽  
Method Development ◽  
Hplc Method ◽  
Column Temperature ◽  
Related Substances ◽  
Rp Hplc ◽  
Ich Guidelines ◽  
Wide Range ◽  
Method Development And Validation ◽  
Development And Validation

A simple, precise and reproducible RP-HPLC method was developed for the estimation of related substances in tilorone dihydrochloride. Quantification was performed using a Zorbax SB-phenyl column (150 × 4.6mm, 5µ) with mobile phase A: 20mM potassium dihydro phosphate + 2ml of triethylamine, pH 2.30 and mobile phase B: acetonitrile, methanol and water 60: 20: 20% v/v. A gradient program was followed with a run time of 55 minutes at a flow rate of 1.0 ml/min. The column temperature was maintained at 40°C, the injection volume was 10 µl and the detection was performed at 269nm using a PDA detector. The retention time of Tilorone dihydrochloride was found to be 10.36 minutes. The proposed method has been validated according to the ICH guidelines for Linearity, Precision, Accuracy, LOD, and LOQ. The method was linear from 0.157 - 3.934μg/ml for standard, 0.153-3.820μg/ml and 0.166 - 4.140μg/ml for impurities, TLHC01 and TLHC02 respectively. The impurities TLHC01 and TLHC02 have been mapped in all stress conditions. The LOD and LOQ of TLHC01 were found at 1.757μg/ml and 5.857μg/ml and 1.919μg/ml and 6.396μg/ml respectively for TLHC02 respectively. Statistical analysis showed that the method was precision, reproducible, selective, specific and accurate for the analysis of Tilorone dihydrochloride and its impurities. The wide range of linearity, sensitivity, precision, short retention times and simple mobile phase have shown that the method is suitable for the routine quantification of mass impurities of tilorone hydrochloride and its dosage pharmaceutical forms with high precision and accuracy.

scholarly journals Analytical method development and validation of Amlodipine besylate in tablet dosage form

2019 ◽  
Vol 9 (4-A) ◽  
pp. 463-466
Author(s):  
Sunil Kumar ◽  
Bigan Ram
Keyword(s):  
Analytical Method ◽  
Mobile Phase ◽  
Method Development ◽  
Amlodipine Besylate ◽  
Ich Guidelines ◽  
System Suitability ◽  
Method Development And Validation ◽  
Development And Validation ◽  
Tablet Dosage

The  accurate and precise HPLC analytical method validated for the determination of Amlodipine besylate  in pharmaceutical dosage form.The chromatographic separation is carried out on shimadzu HPLC system (LC-2010 CHT)  with  UV Vissible  detector and C18(150mm x3.9 mm) 5 μm Column. The Mobile phase consists of Acetonitrile: Methanol: PH 3.0 Buffer (15 V: 35 V: 50 V) , at the flow rate  of  1.0 ml/min and elutes were monitoring  at 237 nm. The observed retention time for Amlodipine besylate was 10.8 min. The % RSD for system precision was 0.41 % and Method precision was 0.58 %.  The method was found to linear (R=0.99996) in the Concentration range of 35-105 μg/ml (50 to 150%). The accuracy was in between 99.50-99.91%. Keywords:  HPLC, Correlation coefficient, System suitability, Bias, % RSD and ICH guidelines

scholarly journals RP-HPLC method development and validation for estimation of rivaroxaban in pharmaceutical dosage forms

2013 ◽  
Vol 49 (2) ◽  
pp. 359-366 ◽  
Author(s):  
Mustafa Çelebier ◽  
Tuba Reçber ◽  
Engin Koçak ◽  
Sacide Altinöz
Keyword(s):  
Method Development ◽  
Internal Standard ◽  
Hplc Method ◽  
Pharmaceutical Dosage Forms ◽  
Rp Hplc ◽  
Ich Guidelines ◽  
Method Development And Validation ◽  
Hplc Method Development ◽  
Development And Validation ◽  
Tablet Dosage

Rivaroxaban, an anti-clotting medication, acts at a crucial point in the blood-clotting process and stops the formation of blood clots. In this study, RP-HPLC method was developed for the determination of rivaroxaban in tablets (Xarelto® (10 mg)). Phenomenex Luna 5 µm C18 100 Å LC Column (250 x 4.6 mm) was used at 40 ºC. Isocratic elution was performed with ACN:Water (55:45 v/v) mixture. The flow rate was 1.2 mL min-1 and UV detection was at 249 nm. Internal standard (Caffeine) and rivaroxaban were eluted within 2.21 and 3.37 minutes, respectively. The developed method was validated according to the ICH guidelines and found to be linear within the range 0.005 - 40.0 µg mL-1. The method was accurate, precise, robust and rapid. Thus, it was applied successfully for the quality control assay of rivaroxaban in tablet dosage form.

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