Development and Validation of a RP-HPLC Method for Simultaneous Estimation of Duloxetine and Methylcobalamin in Bulk and Tablet Dosage Form | Chapter 6 | Pharmaceutical Science: New Insights and Developments Vol. 7

 

A simple, robust, precise, and accurate stability-indicating reverse-phase high-performance liquid chromatographic (RP-HPLC) method was successfully developed and validated for the simultaneous estimation of Duloxetine (DLU) and Methylcobalamin (MCB) in their combined pharmaceutical dosage form. The chromatographic analysis was performed on an Inertsil C18 column with dimensions 4.6 × 250 mm and particle size 5 µm, utilising an isocratic elution technique. The mobile phase consisted of a phosphate buffer adjusted to pH 4.5, which facilitated adequate separation of the analytes. The flow rate of the mobile phase was maintained at 1.0 mL/min, and detection of the eluted components was carried out at a wavelength of 255.0 nm using a UV detector. Under the optimised chromatographic conditions, Duloxetine and Methylcobalamin were eluted at retention times of approximately 5.32 minutes and 3.59 minutes, respectively. The developed method showed excellent linearity over the concentration ranges of 20–120 µg/mL for Duloxetine and 10–60 µg/mL for Methylcobalamin. The correlation coefficients (r²) for both analytes were found to be 0.999, indicating a strong linear relationship between peak area and concentration within the specified ranges. Method accuracy was assessed by recovery studies, which demonstrated mean percentage recoveries of 99.68% for Duloxetine and 100.3% for Methylcobalamin, confirming the accuracy of the method. The relative standard deviation (RSD) values for both analytes in recovery studies were found to be not more than 2% (NMT 2%), reflecting high precision and reproducibility of the method. Precision was further evaluated by conducting intra-day and inter-day studies, both of which showed RSD values within acceptable limits (NMT 2%) for both drugs, supporting the reliability and repeatability of the method over different days and time intervals.

 

The developed RP-HPLC method was validated as per the International Council for Harmonisation (ICH) guidelines, ensuring that all critical parameters, including specificity, linearity, accuracy, precision, robustness, and system suitability, were thoroughly assessed and met the established acceptance criteria. The proposed method is therefore considered suitable for the routine quality control and stability analysis of Duloxetine and Methylcobalamin in their combined dosage forms.

 

Author(s) Details

Kandiboti Lavanya
Department of Pharmaceutical Analysis, Sir C. R. Reddy College of Pharmaceutical Sciences, Eluru, Andhra Pradesh, India.

 

V. Anitha Kumari
Department of Pharmaceutical Analysis, Sir C. R. Reddy College of Pharmaceutical Sciences, Eluru, Andhra Pradesh, India.

 

V. Srinivasa Rao
Department of Pharmacy Practice, Lydia College of Pharmacy, Ravulapalem, Andhra Pradesh, India.

 

Please see the book here:- https://doi.org/10.9734/bpi/psnid/v7/5962

LC-Based Quantification of Diastereomeric Impurities in Entecavir Drug Substances | Chapter 2 | Pharmaceutical Research: Recent Advances and Trends Vol. 8

This chapter describes a simple, sensitive, and cost-effective mobile phase method for determination and quantitation of diastereomeric impurities of Entecavir in drug substances and drug products. Effective chromatographic separation was achieved on a C18 stationary phase (150 x 4.6 mm, 3.5 microns particles) with the economical and simple mobile phase combination such as water and acetonitrile in the ratio of 95:5 (% v/v) delivered in an isocratic mode at a flow rate of 1.0 mL/min at 254 nm. In the developed method, the resolution between Entecavir and its diastereomeric impurities were found to be greater than 2.0. The linearity of the method was demonstrated by means of correlation Co-efficient square (r2) value for Entecavir and its diastereomeric impurities were found to be greater than 0.999. The limit of detection for imp-1, imp-2, imp-3 and Entecavir were 0.002%, 0.002%, 0.003% and 0.008% and the limit of quantification for imp-1, imp-2, imp-3 and Entecavir were 0.007%, 0.006%, 0.008% and 0.025% respectively. The %recovery for imp-1, imp-2, imp-3 were observed in the range between 95 and 105%. The test solution was found to be stable in the diluent for 48 h. The drug was subjected to stress conditions. The mass balance was found close to 99.5%.

 

Author (s) Details

N Balaji
Analytical Development Laboratory, Apicore LLC, New Jersey, USA.

 

Sayeeda Sultana
Department of Chemistry, St. Peter’s University, Avadi, Chennai- 600 054, Tamil Nadu, India.

 

Please see the book here:- https://doi.org/10.9734/bpi/prrat/v8/2720

RP-HPLC Method Development and Validation of Stability Indicating Assay for Simultaneous Determination of Pantoprazole, Diclofenac, Chlorzoxazone in Pharmaceutical Dosage Form | Chapter 6 | Pharmaceutical Science: New Insights and Developments Vol. 1

Background: High-performance liquid chromatography (HPLC) is the fastest-growing analytical technique for the analysis of drugs. Its simplicity, high specificity and wide range of sensitivity make it ideal for the analysis of many drugs in both dosage forms and biological fluids.

Objective: A simple, accurate, precise method was developed, for the simultaneous estimation of the Chlorzoxazone, Pantoprazole, and Diclofenac in solid dosage form.

Method: The chemicals used were Water-HPLC grade, Acetonitrile, Triethylamine, Potassium dihydrogen orthophosphate, and Orthophosphoric acid. Chromatogram was run through BDS C18150×4.6mm, 5m. Mobile phase containing 0.01 % KH₂PO₄ and Acetonitrile in the ratio of 52:48 v/v was pumped through column at a flow rate of 1.0ml/min. The buffer used in this method was 0.01% KH₂P_O4, Temperature was maintained at 30°C. The optimized wavelength for Phar Chlorzoxazone, Pantoprazole, and Diclofenac was 229.0 nm.

Results: In the estimation of the three drugs, four trials were conducted using various solvent systems, columns, and experimental conditions. The retention time of Chlorzoxazone, Pantoprazole, and Diclofenac were found to be 2.229 min, 2.958 min, and 3.568 min. The percent RSD of system precision for Chlorzoxazone, Pantoprazole and Diclofenac were 0.9,0.6 And 0.6, respectively. The percent RSD of the method, Pantoprazole and Diclofenac were found to be 0.6, 1.0 and 0.7 respectively. The percent recovery was obtained as 99.86%, 100.07% and 99.70% for Chlorzoxazone, Pantoprazole, and Diclofenac respectively. LOD values obtained from regression equations of Chlorzoxazone, Pantoprazole and Diclofenac were 0.14 ppm, 0.24 ppm, and 1.83 pm, and LOQ values obtained from regression equations of Chlorzoxazone, Pantoprazole and Diclofenac were 0.42 ppm, 0.72 pm, 5.53 ppm respectively. The regression equation of Chlorzoxazone was y = 8321.9.x + 1397.8 Pantoprazole was y = 9806.1x +6071.7 and of Diclofenac was y = 2575x + 4338.4.

Conclusion: Sensitive detectors have transformed liquid column chromatography into high speed, efficient, accurate and highly resolved methods of separation. Retention times were decreased so that the method developed was simple and economical hence it can be used in regular Quality control tests in industries.

 

Author (s) Details

 

Padmavathi Sakinala
Department of Pharmaceutical Chemistry & Phytochemistry, Pharmaceutical Analysis, Nirmala College of Pharmacy, Atmakur, Mangalagiri, Guntur, AP- 522503, India.

 

Harini Vahika
Department of Analysis, Nirmala College of Pharmacy, Atmakur, Mangalagiri, Guntur, AP, India.

 

Ramu Bhadrama Raju
Department of Chemistry, Madhira Institute of Technology and Science, India.

 

Yeellanki Krishnaveni
Department of Pharmacognosy, Madhira Institure of Science & Technology, India.

 

K. Santhosh
Department of Analysis, Nirmala College of Pharmacy, Atmakur, Mangalagiri, Guntur, AP, India.

 

Sandeep Attinti
Department of Analysis, Nirmala College of Pharmacy, Atmakur, Mangalagiri, Guntur, AP, India.

 

Please see the book here:- https://doi.org/10.9734/bpi/psnid/v1/3081

Analytical Method Development and Validation of Triamcinolone Acetonide by Using RP-HPLC Technique | Chapter 1 | Current Innovations in Chemical and Materials Sciences Vol. 8

The aim of this study primarily focuses on the analytical Method Development and Validation of Triamcinolone Acetonide by using RP-HPLC Technique. Triamcinolone acetonide is a Glucocorticosteroid with great immunosuppressive and anti-inflammatory activity used in the treatment of redness, itching, scaling, crusting like inflammatory skin disorders, and other conditions like dryness with psoriasis on the skin.  The proposed method is an economic and highly sensitive, Reverse Phase High Performance Liquid Chromatographic method for quantification of Triamcinolone acetonide is an active Pharma ingredient (API). The efficient separation was done by using X-bridge phenyl column has a stationary phase and a mobile phase of 50:50 v/v of acetonitrile with Octane sulphonic acid as a buffer solution to adjust the desirable pH-2.5 condition by employing ortho phosphoric acid. The efficient separation of Triamcinolone acetonide was eluted at 6.22 min and its UV absorption was done at 235 nano meters at input flow rate of 1ml/min with Photodiode Array Detector. All the results are acceptable limits with respect to ICH guidelines and the linearity results of Triamcinolone acetonide gave regression equation y= 43591x+14344 and correlation coefficient is (R2) 0.9997. The % RSD is 0.24 for intra-day precision and 0.65 for inter-day precision supports the ruggedness and the proposed approach is eco-friendly by AGREE-Analytical GREEnness metric shows 0.72. The quantification and appropriateness of the method was studied by the various testing parameters like recovery test, fidelity, accuracy, Robustness, and stability of the solution, one can understand the correctness of the approach.

Author(s) Details:

Veeraswami Boddu,
Department of Chemistry, GITAM School of Science, GITAM Deemed to be University, Visakhapatnam, PIN-530045, India.

Kasinath Baratam,
Kasinath Baratam, Syner-G Biopharma Group, Chennai, Tamil Nadu, India.

Please see the link here: https://stm.bookpi.org/CICMS-V8/article/view/14087

Bioanalytical Method Development and Validation of Garenoxacin Mesylate in Human Plasma by RP-HPLC and Its Pharmacokinetic Application | Chapter 9 | Advanced Concepts in Pharmaceutical Research Vol. 7

A simple, precise, accurate RP-HPLC method was developed for the estimation of Garenoxacin mesylate in human plasma using Ciprofloxacin Hydrochloride as an internal standard. The chromatographic conditions optimized were Zorbax Eclipse XDB C18 (250 x 4.6 mm, 5µ) column, Mobile phase 0.1% OrthoPhosphoric Acid and Acetonitrile in the ratio of 50:50 (% v/v) with a flow rate of 1.0 ml/min and injection volume of 50 µL. The detection wavelength was set to 240 nm with a column temperature of 30°C. The retention time of Garenoxacin mesylate was found to be 4.0 min. % Coefficient of Variation of Garenoxacin mesylate was found to be 4.30. % Recovery was obtained as 98.97%. The linearity of the proposed method was established in the concentration range of 0.04 to 4 µg/ml (Correlation Coefficient = 0.999). The lower limit of quantification was 0.04 µg/ml which reached the level of a drug possibly found in human plasma. Further, the reported method was validated as per the ICH guidelines and found to be well within the acceptable range. The method was successfully applied to a pharmacokinetic study after oral administration of immediate-release Zinox tablets (200 mg) in healthy Albino rabbits. The mean Cmax was found to be 5540 ng/ml, which occurred at a Tmax of 1.00 hr. The half-life and AUC0-α values were found to be 13.52 hr and 72187 ng. hr/ml. The method was found to be applicable to bioequivalence studies.

Author(s) Details:

A. Ajitha,
Department of Pharmaceutical Chemistry, Faculty of Pharmacy, Sri Ramachandra Institute of Higher Education and Research (Deemed to be University), No.1 Ramachandra Nagar, Porur, Chennai - 600 116, India.

K. Sujatha,
Department of Pharmaceutical Chemistry, Faculty of Pharmacy, Sri Ramachandra Institute of Higher Education and Research (Deemed to be University), No.1 Ramachandra Nagar, Porur, Chennai - 600 116, India.

Please see the link here: https://stm.bookpi.org/ACPR-V7/article/view/13733

Recent Development and Validation of Tolperisone HCl and Diclofenac Sodium in Bulk and Pharmaceutical Dosage Forms by Using RP HPLC Method | Chapter 5 | Advanced Concepts in Pharmaceutical Research Vol. 7

 High-performance liquid chromatography is at present one of the most sophisticated tools for analysis. The estimation of Tolperisone HCl and Diclofenac sodium was done by RP-HPLC. Tolperisone is an oral, centrally-acting muscle relaxant.  The Phosphate buffer was pH 3.0 and the mobile phase was optimized consisting of Methanol: Phosphate buffer mixed in the ratio of 70:30% v/ v. Inertsil C18 column C18 (4.6 x 150mm, 5µm) or equivalent chemically bonded to porous silica particles was used as stationary phase. The detection was carried out using a UV detector at 260 nm. The samples are weighed using the Afcoset ER-200A weighing balance. The solutions were chromatographed at a constant flow rate of 0.8 ml/min. the linearity range of Tolperisone HCl and Diclofenac sodium was found to be from 100-500 µg/ml of Tolperisone hcl and 1-5µg/ml of Diclofenac sodium. The linear regression coefficient was not more than 0. 999. The values of % RSD are less than 2% indicating the accuracy and precision of the method. The percentage recovery varies from 98-102% of Tolperisone HCl Diclofenac sodium. LOD and LOQ were found to be within the limit. The results obtained on the validation parameters met ICH and USP requirements.

Author(s) Details:

M. Archana,
School of Pharmaceutical Sciences, Vels Institute of Science, Technology and Advanced Studies, PV Vaithiyalingam Rd., Velan Nagar, Krishnapuram, Pallavaram, Chennai, Tamil Nadu – 600043, India.

M. Sumithra,
School of Pharmaceutical Sciences, Vels Institute of Science, Technology and Advanced Studies, PV Vaithiyalingam Rd., Velan Nagar, Krishnapuram, Pallavaram, Chennai, Tamil Nadu – 600043, India.

Please see the link here: https://stm.bookpi.org/ACPR-V7/article/view/13543

Efficient RP-HPLC Method Development for Analysis and accurate Quantification of Specific Anti-Hypertensive Agents in Pharmaceutical Dosage Forms | Chapter 11 | Advanced Concepts in Pharmaceutical Research Vol. 6

This research paper presents the development and validation of a rapid, precise, and economical reversed-phase liquid chromatographic method for simultaneous quantification of four anti-hypertensive agents (ATN, MET, HZT, and AML) and a validated analytical method for the combination of ATN with AML in tablet dosage form. The method, based on a C18 column with optimized conditions, demonstrated well-resolved peaks, good symmetry, and minimal tailing. Validation according to ICH guidelines confirmed specificity, linearity, precision, accuracy, and robustness, with LOD and LOQ values indicating high sensitivity. The proposed method was successfully applied to quantify drug levels in a commercial formulation, with mean assay values within acceptable limits. The study addresses the inadequacies of existing methods, providing a valuable contribution to analytical techniques for anti-hypertensive drug analysis.

Author(s) Details:

Panchumarthy Ravisankar,
Vignan Pharmacy College, Vadlamudi, Guntur-522 213, A.P, India.

Ch. V. Prasada Rao,
Vignan Pharmacy College, Vadlamudi, Guntur-522 213, A.P, India.

A. Viswanath,
Vignan Pharmacy College, Vadlamudi, Guntur-522 213, A.P, India.

B. Divya,
Vignan Pharmacy College, Vadlamudi, Guntur-522 213, A.P, India.

Please see the link here: https://stm.bookpi.org/ACPR-V6/article/view/13478

Exploration and Validation of an Advanced Reverse-Phase HPLC Approach for the Concurrent Analysis of Empagliflozin, Linagliptin, and Metformin in Pharmaceutical Dosage Forms | Chapter 6 | Advanced Concepts in Pharmaceutical Research Vol. 6

A straightforward, precise, and reversed-phase high-performance liquid chromatographic (RP-HPLC) method has been developed and validated for the simultaneous quantification of EMPA, LINA, and MET in pharmaceutical dosage forms. Chromatographic separation was conducted using an Eclipse XDB C18 Column (250 mm × 4.6 mm i.d., particle size 5 µm, maintained at ambient temperature), with a mobile phase consisting of 0.01 N KH2PO4 and acetonitrile in a 50:50 v/v ratio. A pH 5.3 buffer, adjusted with o-phosphoric acid, was utilized. UV detection was carried out at 220 nm, and the retention times were 2.767, 2.362, and 3.276 minutes for EMPA, LINA, and MET, respectively. Calibration plots demonstrated linearity (r2 > 0.999) over the concentration range of 2.5-15 µg/mL for EMPA, 1.25-7.5 µg/mL for LINA, and 250-1500 µg/mL for MET. The method underwent rigorous validation for accuracy, precision, specificity, linearity, and sensitivity. Successfully applied to the quantitative analysis of pharmaceutical dosage forms, the method exhibited no interference from any component of the pharmaceutical dosage form.

Validation studies affirmed the specificity, rapidity, reliability, and reproducibility of the method. High recovery and low relative standard deviation further affirmed the method's suitability for the routine determination of EMPA, LINA, and MET in pharmaceutical dosage forms.

Author(s) Details:

Panchumarthy Ravisankar,
Department of Pharmaceutical Analysis, Vignan Pharmacy College, Vadlamudi, Guntur District – 522 213, Andhra Pradesh, India.

Ch. V. Prasada Rao,
Department of Pharmaceutics, Vignan Pharmacy College, Vadlamudi, Guntur, District – 522 213, Andhra Pradesh, India.

Please see the link here: https://stm.bookpi.org/ACPR-V6/article/view/13416

Estimation of Vinblastine in Pharmaceutical Formulations by RP-HPLC Method | Chapter 12 | Advanced Concepts in Pharmaceutical Research Vol. 4

Vinblastine, a Vinka alkaloid and a synthetic analogue of vincristine is generally secondhand in combination analysis with synthetic fragments. A new simple, exact and accurate reverse phase HPLC order was developed and ratified for the estimation of vinblastine in pharmaceutical formulations utilizing the mobile aspect 90% methanol, 5% acetonitrile and 5% of 0.1% orthophosphoric acid and the pH was maintained at 3.5. Reasoning was carried out utilizing PEAK 7000 isocratic HPLC with rheodyne manual sample injector with a switch (77251). The effect chromatogram obtained has a extreme resolution and low following factor (1.29). The extent of object curve showed a correlation cooperative (r2) of 0.999 for a wide range of drug concentrations of 3-15 ppm. The form was also validated in respect of accuracy, accuracy and particularity. The applicability of the method was too tested accompanying commercial sample of Cytoblastin. This method is more correct, precise and available in terms of linearity, veracity, precision, and so forth.

Author(s) Details:

P. Rama Krishna Veni,
Department of Applied Sciences and Humanities, Sasi Institute of Technology & Engineering, Tadepalligudem - 534101, Andhra Pradesh, India.

N. Sharmila,
Department of Chemistry, Acharya Nagarjuna University, Nagarjuna Nagar, Guntur - 522510, Andhra Pradesh, India.

B. Hari Babu,
Department of Chemistry, Acharya Nagarjuna University, Nagarjuna Nagar, Guntur - 522510, Andhra Pradesh, India.

Please see the link here: https://stm.bookpi.org/ACPR-V4/article/view/13007

Development and Validation of a HPLC Method for the Simultaneous Estimation of Simvastatin and Metformin | Chapter 10 | Advanced Concepts in Pharmaceutical Research Vol. 3

 Simvastatin is individual of the well-known statins that is a HMG-COA reductase inhibitor. Metformin hydrochloride is a well- known spoken antihyperglycemic drug. The present work has created and validated a precise and correct reverse phase liquid chromatographic means for the simultaneous estimation of simvastatin and metformin. This is cause the reversed step HPLC method is ultimate suitable for assessing two together ingredients happening at about the same time. The method was created utilizing a Jasco Auto polltaker HPLC with 50mM Sodium Dihydrogen Phosphate Monohydrate at pH 3.0 and Acetonitrile (30:70 v/v). UV-visible detectors were secondhand for the analysis, and 235 nm was used to monitor the eluents. Simvastatin and metformin were proved to have retention opportunities of 7.650 and 2.858 minutes, respectively. The approach was corroborated in terms of time, robustness, precision, and veracity. The planned method for the simultaneous quantitative perseverance was implemented efficiently.

Author(s) Details:

R. Varade,
Pacific University, Udaipur, Rajasthan, 313024, India.

H. Mishra,
K. J. Somaiya Institute of Engineering and Information Technology, Mumbai, MH, 400022, India.

Please see the link here: https://stm.bookpi.org/ACPR-V3/article/view/12703

HPLC Methods for the Quantification of Cyproheptadine Hydrochloride, Vitamins Using RP-HPLC with UV Detection | Chapter 6 | Advanced Concepts in Pharmaceutical Research Vol. 2

 For the purposes concerning this investigation, we have forged straightforward RP-HPLC methods for the analysis of cyproheptadine hydrochloride, thiamine mononitrate, calcium pantothenate, and pyridoxine hydrochloride. The International Conference on Harmonization's (ICH) Q2(R1) 2005 tests were followed in the conduct concerning this study. The quality control of various APIs in single dose forms depends massively on the availability of reliable, high-throughput examining technologies. Here, we present the growth and validation of two methods for the identification and calculation of calcium pantothenate, cyproheptadine hydrochloride (CH), thiamine mononitrate (Vit. B1), and pyridoxine hydrochloride (Vit. B6) in uncoated tablets. For the vitamin test, a movable phase combination of phosphate buffer pH 3.5 and flammable liquid in the ratio 93:7 was secondhand. The stationary point used was Eurospher ODS (150 x 4.5mm), and the flow rate was judge 1.0 mL/min (ambient hotness settings). For thiamine mononitrate and pyridoxine hydrochloride, the awareness of detection was 270 nm accompanying a run time of 0.00 to 5.50 summary, and for calcium pantothenate, it was 205 nm with a run occasion of 5.50 to 11.00 minutes. The dose volume was 20 µL. A good judgment, and a short run time of 11 record were achieved accompanying the validated environments. The retention opportunities of thiamine mononitrate, pyridoxine hydrochloride and calcium pantothenate were 2.823 ± 0.020, 4.184 ± 0.007 and 10.025 ± 0.015 minutes individually.The mobile phase arrangement for cyproheptadine HCl was methanol and an ion-making solution (70:30), judge a flow rate of 1.0 mL/min, a runtime of 8 notes of meeting, an injection capacity of 20 µL, and a wavelength of 285 nm utilizing Eurospher ODS (150 x 4.5 mm) as the stationary chapter. The retention opportunity for cyproheptadine HCl was 4.961 ± 0.006.Both methods were raise to be distinguishing, with undeviating dynamic ranges of 0.0192 mg/mL - 0.0288 mg/mL for thiamine mononitrate, 0.0128 - 0.0192 mg/mL for pyridoxine hydrochloride, 0.032 - 0.048 mg/mL for calcium pantothenate and 0.032 - 0.048 mg/mL for cyproheptadine hydrochloride. The equivalence coefficient (R2) for cyproheptadine hydrochloride, thiamine mononitrate, pyridoxine hydrochloride and calcium pantothenate were more 0.999.The purpose of this study was to evolve and validate plain HPLC methods for the belief of cyproheptadine hydrochloride, vitamins B1, B5 and B6 in combined portion of drug or other consumable forms. The proposed means were found expected precise, correct, and robust for the belief of cyproheptadine hydrochloride, vitamins B1, B5 and B6.

Author(s) Details:

Yayra Tuani,
Letap Pharmaceuticals Ltd., P.O. Box GP 3346, Accra, Ghana.

Seth Amo-Koi,
United States Pharmacopeia-Ghana, No. 3 Park Avenue, Motorway Extension, North Dzorwulu, P.O. Box WY 1204, Kwabenya, Accra, Ghana.

David Mingle,
Department of Pharmaceutical Sciences, College of Pharmacy, University of Tennessee Health Science Centre, 881 Madison Ave, Memphis, TN 38163, USA.

Andrew Gordon,
Department of Science Laboratory Technology, Accra Technical University, Accra, Ghana.

Angela Asor,
Department of Chemistry, Michigan State University, 578 S Shaw Lane, East Lansing, MI 48824, USA.

Please see the link here: https://stm.bookpi.org/ACPR-V2/article/view/12338

Analytical Method Development and Validation of Simultaneous Estimation of Ivermectin and Albendazole Byusing RP-HPLC | Chapter 6 | Novel Aspects on Chemistry and Biochemistry Vol. 7

 A new arrangement was established for concurrent estimation of Ivermectin and Albendazole by RP-HPLC method. The chromatographic environments were successfully grown for the separation of Ivermectin and Albendazole by utilizing ACE C18 column (4.6×150 mm) 5µ, flow rate was 1.2 ml/min, travelling phase percentage was (70:30 v/v) methanol: Phosphate safeguard pH 3 (pH was adjusted with ortho phosphoricacid), discovery wavelength was 240 nm. The means used was WATERS HPLC Auto Sampler, Separation piece 2690, photodiode array detector 996, Empower-software variant-2. The retention periods were found expected 2.344 mins and 3.284 mins. The % purity of Ivermectin and Albendazole was found expected 101.27% and 99.97% respectively. The system rightness parameters for Ivermectin and Albendazole such as hypothetical plates and tailing determinant were found expected 4668, 1.3 and 6089 and 1.2, the resolution was found expected 6.0. The analytical means was validated in accordance with ICH guidelines (ICH, Q2 (R1)). The linearity study n Ivermectin and Albendazole was in the direction of concentration range of 50 µg-250 µg and 5µg-50µg and equivalence coefficient (r2) was erect to be 0.999 and 0.999, % recovery was erect to be 99.56% and 99.48%, % RSD for repeatability was0.2 and 0.2, % RSD for middle precision was 0.2 and 0.1respectively. The accuracy study was precise, robust, and repeatable.  LOD profit was 3.17 and 5.68, and LOQ value was 0.0172 and 0.2125 individually. Hence the suggested RP-HPLC pattern can be used for routine reasoning of Ivermectin and Albendazole in API and Pharmaceutical dosage form.

Author(s) Details:

Meruva Sathish Kumar,
MNR College of Pharmacy, Fasalwadi, Sangareddy, India.

Phani Deepika Polampalli,
MNR College of Pharmacy, Fasalwadi, Sangareddy, India.

Bandi Narendar,
MNR College of Pharmacy, Fasalwadi, Sangareddy, India.

S. Siva Prasad,
MNR College of Pharmacy, Fasalwadi, Sangareddy, India.

Rasapally Ramesh Kumar,
MLR College of Pharmacy, Dundigal, India.

Please see the link here: https://stm.bookpi.org/NACB-V7/article/view/11964

Rapid Determination of Carboplatin and Docetaxel Using RP-HPLC with PDA Detector | Chapter 11 | Novel Aspects on Pharmaceutical Research Vol. 7

 Objective: In the current inquiry, to separated and legalize the cancer healing drugs (Carboplatin and Docetaxel) through the HPLC (e-2695) tool containing a PDA indicator.Methods: A simple, discriminating, validated and well-defined establishment that shows isocratic RP-HPLC methodology for the determinable determination of Carboplatin and Docetaxel. The chromatographic strategy exploited Symmetry C18 column of ranges 150x4.6 mm, 3.5 micron, using isocratic elution accompanying a mobile phase of acetonitrile and 0.1% ortho phosphoric acid (40:60). A flow rate of 1 ml/brief time period and a detector intuitiveness of 225 nm utilizing the PDA indicator were given in the instrumental scenes. Recovery, specificity, extent of object, accuracy, robustness, masculinity were determined as any of method confirmation and the results were found to be inside the acceptable range. Validation of the projected method was completed activity according to an international convention on harmonization (ICH) directions.Results: LOD and LOQ for the two alive ingredients were established concerning test concentration. The measurement charts plotted were linear accompanying a regression cooperative of R2>0.999.Conclusion: The proposed form to be fast, simple, possible and affordable in assay condition. During strength tests, it can be secondhand for routine analysis of production samples and to confirm the quality of drug samples all the while stability studies.

Author(s) Details:

Potturi Rama Devi,
Vidya Jyothi Institute of Technology, Hyderabad, Telangana, India.

Kantipudi Rambabu,
RVR & JC College of Engineering, Chowdavaram, Guntur, AP, India.

Please see the link here: https://stm.bookpi.org/NAPR-V7/article/view/11441

The Development and Validation of RP-HPLC Method for Lamivudine, Dolutegravir, and Tenfovir in Human Plasma | Chapter 3 | Novel Aspects on Pharmaceutical Research Vol. 2

 The present work proposed to develop a plain, rapid, and correct method for the estimation of Dolutegravir, Lamivudine and Tenofovir disoproxil fumarate cruel plasma, as per US-FDA directions. Moreover and the present form is the first for the estimation concerning this combination in a biological form. For the estimation of Lamivudine, Dolutegravir, and Tenfovir disoproxil fumarate cruel plasma utilizing the Cobicistat as internal standard by RP-HPLC (Reverse Phase-High Performance Liquid Chromatographic) method, a straightforward, precise, and correct method has existed developed. The clean drug samples of Dolutegravir, Lamivudine and Tenofovir in were purchased from Selleck chem LLC provided by Pro lab marketing. HPLC grade Acetonitrile, HPLC grade Methanol in addition other chemical compound were obtained from Merck synthetic division, Mumbai. The Chromatographic break-up was achieved on discovery C18, 250 mm x 4.6 mm, 5μ, Column at 300C hotness.The separation was attained employing a travelling phase resides of 0.1% v/v Ortho phosphoric acid and Acetonitrile taken in the ratio of 65:35 (v/v). The flow rate was uphold at 1.0 ml/min, discovery wave length was 277 nm. Retention period of Lamivudine, Dolutegravir and Tenfovir were found expected 2.994 min, 4.350 min and 5.688 brief time period respectively. The peaks were raise to be innocent interference. The order was validated over a dynamic uninterrupted range of 60-2400 ng/ml, 190-7600 ng/ml, and 18-720 ng/ml for Lamivudine, Dolutegravir and Tenfovir respectively, accompanying a Correlation coefficient of 0.998. The accuracy and accuracy of samples of six copy measurements at lower limits of quantification level were believable. The analytes were found expected stable cruel plasma at -28°C for 37 days. The decision of Lamivudine, Dolutegravir, and Tenfovirin in human plasma is appropriate on account of the stability, nervousness, specificity, and reproducibility concerning this method. According to US-Food and Drug Administration directions, the reported method was certified, and it was discovered expected substantially inside the acceptable range.

Author(s) Details:

Padmavathi Sakinala,
Department of Pharmaceutical Analysis, Nirmala College of Pharmacy, Atmakur, Mangalagiri, Guntur, AP-522503, India.

Shaik Abdul Rahaman,
Department of Pharmaceutical Analysis, Nirmala College of Pharmacy, Atmakur, Mangalagiri, Guntur, AP-522503, India.

J. Naga Sharmila,
Department of Pharmaceutical Analysis, Nirmala College of Pharmacy, Atmakur, Mangalagiri, Guntur, AP-522503, India.

M. Sireesha,
Department of Pharmaceutical Analysis, Nirmala College of Pharmacy, Atmakur, Mangalagiri, Guntur, AP-522503, India.

G. Pujitha,
Department of Pharmaceutical Analysis, Nirmala College of Pharmacy, Atmakur, Mangalagiri, Guntur, AP-522503, India.

Please see the link here: https://stm.bookpi.org/NAPR-V2/article/view/10596

Estimation of Ribociclib and Letrozole in Solid Dosage form (Tablet): A Novel Analytical Method | Chapter 9 | Current Overview on Pharmaceutical Science Vol. 9

An attempt was created to develop a plain, rapid, and corroborated method for the concurrent estimation of ribociclib and letrozole together tablet portion of drug or other consumable form.Inhibitors of cyclin D1/CDK4 (Cyclin-dependent kinase 4) [2] and CDK6 (Cyclin-weak kinase 6) [2] are found in Ribociclib, which is retailed by Novartis under the brand names Kisqali and Kryxana. This drug is used to treat some types of feelings cancer. The mixture of aromatase inhibitors and fulvestrant Inhibitors of cyclin D1/CDK4 (Cyclin-dependent kinase 4) and CDK6 (Cyclin-reliant kinase 6) are found in Ribociclib, This drug is used to treat few types of breast malignancy. The combination of aromatase inhibitors and fulvestrant.The chromatographic break-up was carried out on Waters, proportion C18 (150 mm×4.6 mm with 3.5 µm), travelling phase secondhand was a mixture of safeguard and acetonitrile in the ratio of 80:20, accompanying flow rate of 1ml/min and dose volume of 10 µL for the assay. The detection was finished using PDA at 260 nm, accompanying run time of 5 brief time period. The retention opportunity for the drugs ribociclib and letrozole was detected expected 2.648 min and 3.151 brief time period, respectively. The pattern was validated in accordance with ICH guidelines.The extent of object of letrozole and ribociclib was observed expected in the range of 0.50–7.50 and 40.01–600.15, Correlation coefficient (r2) 0.999 and 0.9983, individually. Accuracy for ribociclib and letrozole is carried out by repeatable concentrations of 50%, 100%, and 150. Validation determinants of robustness and masculinity were detected to be in limits.The grown method was plain, rapid, and logical; it can be secondhand for the simultaneous belief of ribociclib and letrozole tablet portion of drug or other consumable form in routine analysis. The approved method maybe used for the routine reasoning of both the drugs from size and different formulations and will help in healing drug monitoring (TDM) and bioavailability studies.

Author(s) Details:

Bhagyalata Satapathy,
The Tamil Nadu Dr. M.G.R Medical University, India.

Chaitanya Bangari,
The Tamil Nadu Dr. M.G.R Medical University, India.

Please see the link here: https://stm.bookpi.org/COPS-V9/article/view/10178

UV and RP-HPLC Method Development and Validation for Estimation of Cilnidipine| Chapter 7 | Current Overview on Pharmaceutical Science Vol. 3

 The current experiment was devised to develop and endorse a simple RP-HPLC methods for determining Cilnidipine. Cilnidipine was quantified utilizing UV spectroscopy. Action separation of Cilnidipine was realized by using a C18 pillar. Mobile phase blend of methanol: water (90:10 v/v) was pressure at the flow of 1 ml/min. Detection At 241 nm, detection was completed activity. In accordance with the International Conference on Harmonization's (ICH) Q2R1 recommendations, confirmation parameters were determined. With a parametric value (r2) of 0.999, the uniformity curve for cilnidipine was linear over the range of 2–10 mg/ml.  The plan was noticed to be correct (101.66% recovery), exact (intraday, 1.65 and inter epoch, 1.38) and robust (% RSD was premeditated to be 0.66, 0.58 and 0.81 for alternative in mobile phase arrangement, wave length and flow speed respectively) for the reasoning of Cilnidipine. The developed system has successfully achieved all validation tests and can be used to estimate the attendance of cilnidipine in both drug formulations and bulk.

Author(s) Details:

Biswajit Samantaray,
School of Pharmacy and Life Sciences, Centurion University of Technology and Management, Odisha, India.

Satish Kanhar,
School of Pharmacy and Life Sciences, Centurion University of Technology and Management, Odisha, India.

Ashirbad Nanda,
School of Pharmacy and Life Sciences, Centurion University of Technology and Management, Odisha, India.

Please see the link here: https://stm.bookpi.org/COPS-V3/article/view/9112

A Stability Indicating RP-HPLC Method Validation for Simultaneous Estimation of Linagliptin and Empagliflozin in Pharmaceutical Dosage Form | Chapter 12 | Current Aspects in Pharmaceutical Research and Development Vol. 8

 Aims: Linagliptin and Empagliflozin are a new medicine combination for the treatment of Diabetes Mellitus, one of humanity's oldest and most fatal diseases. The goal of this study was to develop and validate a new, quick, sensitive, specific, and stable stability indicating analytical approach for the simultaneous estimation of Linagliptin and Empagliflozin in a fixed dose pharmaceutical dosage form.

Study Design: The ICH guideline "Validation of analytical procedures: Test and Methodology Q2(R1)" was followed for method development and validation.

Methodology: The method was developed using a phenyl column (150mm 4.6 mm, 3.5 mm particle size), a 30°C column temperature, an HPLC system with a PDA detector, and a degassed mixture of 0.1 percent perchloric acid: acetonitrile (75:25 v/v) as the mobile phase. With responses measured at 226 nm, the flow rate was set to 1.2 ml/min, the injection volume was 20 l, and the run time was 22 minutes.

Linagliptin and Empagliflozin had retention times of 10.2 and 15.7 minutes, respectively. With correlation values more than 0.999, linearity was established in the range of 10-30 g/ml for Linagliptin and 20-60 g/ml for Empagliflozin. Linagliptin and Empagliflozin had percentage recoveries of 98.4-100.5 percent and 99.2-100.4 percent, respectively. The International Conference on Harmonization (ICH) Q2 R1 criteria were used to evaluate the validation parameters. HCl, NaOH, H2O2, heat, and UV radiation were used in the forced degradation investigations. The created method was used to perform quantification and hyphenated instrumental analysis with great success.

Conclusion: The developed method's significance lies in the fact that it may be used for routine or unknown sample analysis of Linagliptin and Empagliflozin in pharmaceutical dosage forms offered by diverse pharmaceutical companies.

Author(S) Details

Darshak Patel
Department of Quality Assurance & Pharm. Chem., Faculty of Pharmacy, Nootan Pharmacy College, Sankalchand Patel University, S. K. Campus, Visnagar-384315, Gujarat, India.

Ujashkumar Shah
Department of Quality Assurance & Pharm. Chem., Faculty of Pharmacy, Nootan Pharmacy College, Sankalchand Patel University, S. K. Campus, Visnagar-384315, Gujarat, India.

Jayvadan Patel
Department of Quality Assurance & Pharm. Chem., Faculty of Pharmacy, Nootan Pharmacy College, Sankalchand Patel University, S. K. Campus, Visnagar-384315, Gujarat, India.

Darshana Patel
Department of Quality Assurance & Pharm. Chem., Faculty of Pharmacy, Nootan Pharmacy College, Sankalchand Patel University, S. K. Campus, Visnagar-384315, Gujarat, India.

Pavan Patel
Restech Pharmaceuticals, Plot No. 407 New Ahmedabad Industrial Estate, Sarkhej-Bavala Road, Moraiya-382 210, Dist-Ahmedabad, Gujarat, India.


View Book:- https://stm.bookpi.org/CAPRD-V8/article/view/5653

Study on Development and Validation of Stability Indicating RP-HPLC Method for Guaifenesin | Chapter 1 | Technological Innovation in Pharmaceutical Research Vol. 11

 A simple, accurate, and exact stability indicating RP HPLC technique was developed and validated for the determination of Guaifenesin in bulk and formulation. Under various forced degradation settings, the drug and its breakdown products were separated on a Phenomenex C18 column (250 4.6 mm, 5) using a mobile phase of methanol:water (60:40 percent v/v). The flow rate was kept constant at 1.0 mL/min and the eluents were detected at 230 nm. In forced degradation testing, guaifenesin deteriorated in acid, alkali, photolytic, and wet heat environments, but remained stable in H2O2 (oxidative) and dry heat environments. In calibration curve investigations, linearity was discovered in the concentration range of 2-12 g/mL, with a regression coefficient (R2) of 0.999. y = 102800 x + 24264 was the equation found. For the determination of guaifenesin, a rapid, simple, sensitive, and accurate HPLC –UV approach has been described. It may be deduced from the forced degradation investigations that guaifenesin is degraded by acid, alkali, moist heat, and photolysis.

Author (S) Details

Sandhya R. Gawai
Department of Quality Assurance, MET Institute of Pharmacy, Nasik, Maharashtra, India.

Kiran Gadge
Department of Quality Assurance, MET Institute of Pharmacy, Nasik, Maharashtra, India.

Sandeep Sonwane
Department of Quality Assurance, MET Institute of Pharmacy, Nasik, Maharashtra, India.

View Book :- https://stm.bookpi.org/TIPR-V11/article/view/3123

Development of RP-HPLC Method for Simultaneous Estimation of Metformin and Pioglitazone in Pharmaceutical Formulation | Chapter 11 | Technological Innovation in Pharmaceutical Research Vol. 3

A fast, selective, speedy, accurate, and cost-effective reverse phase HPLC technique has been devised for the simultaneous quantification of metformin and pioglitazone from pharmaceutical dosage forms. The experiment was carried out on a phenomenex C18 column (25 cm x 4.6 mm i.d., 5 mm i.d., 5 mm i.d., 5 mm i.d., 5 mm i.d., 5 mm i.d., 5 mm i.d., phosphate buffer phase containing acetonitrile (adjusted to pH 5.0 using orthophosphoric acid) at a flow rate of 1. ml/min (50:50 v/v). The wavelength of detection was 258 nm. As a measure of internal control, The drug etoricoxib was utilized. The retention times for paracetamol, aceclofenac, and etoricoxib were 4.75, 6.44, and 6.44, respectively. 8.83 minutes and 8.83 minutes, respectively. In terms of precision, linearity, detection limit, and detection limit, The established method was validated in terms of quantitation and solution stability. These medications' dosage forms in combination dosage forms can be calculated using the provided procedure. Raw materials, formulations, and dissolution tests can all be checked using the current RPHPLC equipment.

Author (s) Details

S. Alexandar
Department of Pharmaceutical Chemistry, Vinayaka Mission’s College of Pharmacy, Vinayaka Missions Research Foundation (Deemed to be University), Yercaud Main Road, Salem – 636008, India.

View Book :- https://stm.bookpi.org/TIPR-V3/article/view/1154