scholarly journals Development and validation of a single HPLC method for the determination of thirteen pharmaceuticals in bulk and tablet dosage form

2021 ◽  
Vol 35 (1) ◽  
pp. 17-31
Author(s):  
B. Tegegne ◽  
B. S. Chandravanshi ◽  
F. Zewge ◽  
L. Pillay ◽  
L. Chimuka
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
High Performance ◽  
Dosage Form ◽  
Hplc Method ◽  
Mobile Phase Flow Rate ◽  
Ich Guidelines ◽  
Relative Standard ◽  
Tablet Dosage

The aim of this study was to develop and validate a high performance liquid chromatography (HPLC) method for the determination of thirteen selected pharmaceutical compounds (metformin, amoxicillin, chloroquine, theophylline, trimethoprim, caffeine, norfloxacin, ciprofloxacin, acetylsalicylic acid, doxycycline hyclate, metronidazole, albendazole and cloxacillin) in bulk and tablet dosage form. Chromatographic separation using a Kromasil C18 column, gradient elution with aqueous formic acid (0.1%), methanol and acetonitrile, a UV absorption wavelength of 250 nm and a mobile phase flow rate of 1 mL/min over a 22 min run time was optimized for complete separation of the selected target compounds. The method was validated and results for: linearity, precision, sensitivity, accuracy, specificity, suitability and method robustness were obtained and met the ICH guidelines. Calibration curve correlation coefficients ranged from 0.9985-0.9998 and the percentage relative standard deviations for repeated analysis was below 5%, indicating acceptable method precision. The limits of detection (LODs) and quantification (LOQs) ranged from 0.020-0.27 µg/L and 0.080-0.91 µg/L, respectively. The accuracy study yielded recoveries in the ranges 86.0-102% for pure compounds and 90.9-106% for compounds in tablet dosage form. The method is robust for small or deliberate changes to the chromatographic parameters and found to be appropriate for analysis of tablets for the determination of the thirteen pharmaceuticals.                     KEY WORDS: Pharmaceuticals, Bulk determination, Tablet dosage, High performance liquid chromatography, Method development, ICH guidelines   Bull. Chem. Soc. Ethiop. 2021, 35(1), 17-31. DOI: https://dx.doi.org/10.4314/bcse.v35i1.2

scholarly journals A novel simultaneous high performance liquid chromatography-PDA method for the determination of Tenofovir AF, Darunavir, Emtricitabine and Cobicistat in bulk and its application to marketed formulation

2022 ◽  
Vol 8 (1) ◽  
Author(s):  
Challamalla Pavani ◽  
E. Susithra
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
High Performance ◽  
Dosage Form ◽  
Volume Ratio ◽  
Quantitation Limit ◽  
Ich Guidelines ◽  
Tenofovir Alafenamide ◽  
Tablet Dosage

Abstract Background The present research article involves the simultaneous determination of Tenofovir alafenamide, Darunavir, Emtricitabine and Cobicistat in bulk as well as in tablet dosage form using high performance liquid chromatography. Result The separation was performed using DIKMA Spursil, C18, ODS, (4.6 × 150 mm × 5 µm) analytical column using the mobile phase acetonitrile and 0.1% Orthophosphoric acid in the volume ratio of 70:30 at pH 3. The eluents were detected using PDA detector at 254.0 nm. After optimization subsequent validation study of different parameters was performed by utilizing the optimised condition as per the ICH guidelines. Under this optimised conditions Tenofovir alafenamide, Darunavir, Emtricitabine and Cobicistat were eluted at 2.287 min, 2.507 min, 4.062 min, 6.011 min respectively. Percentage assay was found 99.21% for Tenofovir alafenamide, 99.80% for Darunavir, 99.80% for Emtricitabine and 99.84% for Cobicistat. Tenofovir alafenamide was found linear in the range of 2.0–10.0 µg/mL, Darunavir (160.0–800.0 µg/mL), Emtricitabine (40.0–200.0 µg/mL) and for cobicistat (30.0–150.0 µg/mL). The corelation coefficient was found 0.999 for all the APIs. The detection limit was found 0.14 µg/mL for Tenofovir alafenamide, 2.14 µg/mL for Darunavir, 0.6 µg/mL for Emtricitabine and 7.32 µg/mL for cobicistat. In the LOQ study the quantitation limit was found 0.47 µg/mL for Tenofovir alafenamide, 7.12 µg/mL for Darunavir, 2.10 µg/mL, for Emtricitabine and 24.42 µg/mL for cobicistat. Conclusion All the studied API’s has been highly resolute utilizing the optimised condition and found extremely suitable for the determination of all of them simultaneously in marketed dosage form as well as in the bulk form.

scholarly journals A Selective High-Performance Liquid Chromatography Method for the Determination of Reboxetine in Bulk Drug and Tablets

2006 ◽  
Vol 89 (6) ◽  
pp. 1552-1556
Author(s):  
ArmaĞan Önal ◽  
Olcay SaĞiri ◽  
S Müge Çetin ◽  
Sidika Toker
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
High Performance ◽  
Depressive Disorders ◽  
Degradation Products ◽  
Severe Depression ◽  
Hplc Method ◽  
Chromatography Method ◽  
Relative Standard

Abstract Reboxetine is used as a selective noradrenaline reuptake inhibitor for the treatment of major depressive disorders. It is effective in the treatment of severe depression and safer to use than traditional tricyclic antidepressants. In this study, a novel, simple, and rapid stability-indicating high-performance liquid chromatography (HPLC) method for reboxetine methansulfonate was successfully developed and validated for the assay of tablets. The method was used to quantify reboxetine in tablets; it employed a C18 column (150 4.6 mm id) with an isocratic mobile phase consisting of methanolphosphate buffer (pH 7, 0.02 M; 55 + 45, v/v) at a flow rate of 1.0 μmL/min. Reboxetine was detected by an ultraviolet detector at 277 nm. The retention time of reboxetine was about 4.5 min. The developed HPLC method was validated with respect to linearity, precision, sensitivity, accuracy, and selectivity. The method was linear over the concentration range 150 g/mL (r 0.9999). The limits of detection and the quantitation of reboxetine were 0.1 and 0.3 μg/mL, respectively. The relative standard deviation values for intraday and interday precision were 0.781.01 and 1.081.37%, respectively. Selectivity was validated by subjecting a stock solution of reboxetine to neutral, acid, and alkali hydrolysis, as well as oxidation, dry heat treatment, and photodegradation. The peaks of the degradation products did not interfere with the peak of reboxetine. The results indicated that the proposed method could be used in a stability assay. The proposed method was successfully applied to the determination of reboxetine in tablets. Excipients present in the tablets did not interfere with the analysis.

scholarly journals PENGEMBANGAN DAN VALIDASI METODE KROMATOGRAFI CAIR KINERJA TINGGI (KCKT) UNTUK ESTIMASI KADAR SIMULTAN ANTIEMETIK PIRIDOKSIN HIDROKLORIDA DAN PIRATIAZIN TEOKLAT DALAM BENTUK SEDIAAN TABLET

2019 ◽  
Vol 6 (2) ◽  
pp. 95
Author(s):  
Fikri Alatas ◽  
Hernandi Sujono ◽  
Woro Artati Sucipto
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
High Performance ◽  
Dosage Form ◽  
Ultra Violet ◽  
Hplc Method ◽  
Simultaneous Estimation ◽  
Pyridoxine Hydrochloride ◽  
Development And Validation ◽  
Tablet Dosage

<p align="center"><strong>Abstrak</strong><strong></strong></p><p align="center"><strong> </strong></p><p>Metode kromatografi cair kinerja tinggi (KCKT) dengan detektor ultra lembayung telah dikembangkan dan divalidasi untuk estimasi kadar secara simultan campuran piridoksin hidroklorida (PH) dan piratiazin teoklat (PT)dalam sediaan tablet antiemetik. Proses pemisahan terjadi dalam kolom Inertsil® ODS-3 pada panjang gelombang 280 nm dengan laju alir 1,0 mL/menit. Fase gerak yang optimal untuk pemisahan adalah campuran methanol-asam asetat 1% (20:80) dengan waktu retensi PH dan PT berturut-turut adalah 1,2 dan 9,8 menit. Perolehan kembali PH dan PT berturut-turut adalah 100,13 dan 99,78 %. Batas deteksi untuk PH dan PT berturut-turut adalah 0,21 dan 0,22 µg/mL, sedangkan batas kuantisasinya berturut-turut adalah 0,70 dan  0,72 µg/mL. Metode ini dapat diterapkan sebagai metode untuk estimasi kadar campuran piridoksin hidroklorida dan piratiazin teoklat dalam bentuk sediaan tablet secara simultan.</p><p> </p><p><strong>Kata kunci:</strong> Piridoksin hidroklorida, piratiazin teoklat, KCKT, tablet</p><p> </p><p align="center"><strong><em>Development and validation of high performance liquid chromatography (HPLC) method for simultaneous estimation of antiemetic pyridoxyne hydrochloride and pyrathiazine theoclate in tablet dosage form</em></strong></p><p> </p><p align="center"><strong><em>Abstract</em></strong><strong><em></em></strong></p><p><em> </em></p><p><em>The high performance liquid chromatography (HPLC) method with an ultra violet detector has been developed and validated for simultaneous estimation of pyridoxine hydrochloride (PH) and pyrathiazine theoclate (PT) in antiemetic tablet preparations. The separation process occurs in the Inertsil® ODS-3 column at a wavelength of 280 nm with a flow rate of 1.0 mL /min. The optimal mobile phase for separation is a mixture of methanol-acetic acid 1% (20:80) with the retention times of PH and PT 1.2 and 9.8 minutes respectively. The recoveries of PH and PT were 100.13 and 99.78%, respectively. The detection limits for PH and PT were 0.21 and 0.22 µg / mL respectively, while the quantisation limits were 0.70 and 0.72 µg / mL, respectively. This method can be applied as a method for simultaneous estimating the levels of pyridoxine hydrochloride and pyrathiazine theoclate in tablet dosage form.</em><em></em></p><p><em> </em></p><p><strong><em>Keywords:</em></strong><em> Pyridoxine hydrochloride, pyrathiazine theoclate, HPLC, tablet</em></p>

REVERSE PHASE HIGH PERFORMANCE LIQUID CHROMATOGRAPHIC METHOD FOR DETERMINATION OF REGORAFENIB IN TABLET DOSAGE FORM

INDIAN DRUGS ◽  
2018 ◽  
Vol 55 (06) ◽  
pp. 63-68
Author(s):  
R. Raut ◽  
◽  
A. Patil ◽  
V. K Munipalli ◽  
M. Patel ◽  
...  
Keyword(s):  
High Performance ◽  
Dosage Form ◽  
High Performance Liquid Chromatographic ◽  
Hplc Method ◽  
Control Analysis ◽  
Reverse Phase ◽  
Ich Guidelines ◽  
Tablet Dosage ◽  
Liquid Chromatographic

A simple precise and rapid Reverse Phase High Performance Liquid Chromatographic (RP-HPLC) method has been developed for quantitative determination of Regorafenib in tablet dosage form. In this method Hypersil Gold (C18, 150mm× 4.6mm id, 3μ) column with mobile phase consisting of Trifluoroacetic acid (0.2% v/v) and Acetonitrile in the ratio of (50: 50 v/v) at 400C in an isocratic mode was used. The detection was carried out at 260 nm and 20μL injection volume was selected with the flow rate 1mL/min. The linearity range of Regorafenib shows concentration between 5-200 μg/mL. The regression coefficient obtained was 0.999. Retention time of Regorafenib was found to be 6.49 minutes. Acetonitrile and Water in the ratio of (3:1) was used as a diluent. The method was validated as per ICH guidelines and is simple, fast, accurate, precise and can be applied for routine quality control analysis of Regorafenib in tablet dosage form.

Validation of HPLC Method for Determination of Histamine in Human Immunoglobulin Formulations

2020 ◽  
Vol 103 (5) ◽  
pp. 1223-1229
Author(s):  
Michikazu Tanio ◽  
Toru Nakamura ◽  
Hideki Kusunoki ◽  
Kyohei Ideguchi ◽  
Kazuyuki Nakashima ◽  
...  
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
Standard Deviation ◽  
High Performance ◽  
Gradient Elution ◽  
Hplc Method ◽  
Human Immunoglobulin ◽  
Histamine Dihydrochloride ◽  
Relative Standard

Abstract Background Histamine fixed-immunoglobulin formulations, which consisted of 0.15 µg of histamine dihydrochloride and 12 mg of human immunoglobulin in a vial, are used for anti-allergic treatments, and controlling the amounts of histamine in the formulations is essential to avoid histamine intoxication. Objective A high-performance liquid chromatography (HPLC) method for determination of histamine contents of the formulations was established and validated. Methods Histamine extracted from the formulation was labeled with 6-aminoquinolyl-N-hydroxysuccinimidyl carbamate and was analyzed by gradient elution HPLC with UV detection at 260 nm. Results The method showed linearity in the range 0.8–2.4 µM (R &gt; 0.999), accuracy (100.1–105.8% recovery), and precision (relative standard deviation ≤ 1.93%). The validated method was applied for five lots of the pharmaceutical, and their histamine contents were determined to be 0.149–0.155 µg/vial. Conclusions These results indicated that the validated method is useful to control amounts of histamine in biopharmaceutical products. Highlights The HPLC method was developed for quantitative determination of histamine content of the histamine fixed-immunoglobulin formulations.

scholarly journals ANALYTICAL METHOD DEVELOPMENT AND VALIDATION OF NEW STABILITY-INDICATING REVERSE-PHASE HIGH-PERFORMANCE LIQUID CHROMATOGRAPHY METHOD FOR SIMULTANEOUS ESTIMATION OF METFORMIN HYDROCHLORIDE AND EMPAGLIFLOZIN IN TABLET DOSAGE FORM

2019 ◽  
Vol 12 (1) ◽  
pp. 241 ◽  
Author(s):  
Geetha Susmita A ◽  
Rajitha G ◽  
Ramya Yadav Y ◽  
Uma P
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
High Performance ◽  
Dosage Form ◽  
Simultaneous Estimation ◽  
Reverse Phase ◽  
Stability Indicating ◽  
Rp Hplc ◽  
Relative Standard ◽  
Tablet Dosage

Objective: The objective of this study was to develop and validate a stability-indicating reverse-phase high-performance liquid chromatography (RP-HPLC) method for the simultaneous estimation of the metformin and empagliflozin in tablet dosage forms.Methods: The chromatographic conditions were optimized and it was run through Std. BDS (250 mm × 4.6 mm, 5 m) column with mobile phase consisting of 0.1% orthophosphoric acid buffer: acetonitrile in the ratio of 50:50. The flow rate was 1 ml/min and optimized wavelength was 210 nm. Temperature was maintained at 30°C.Results: The retention times of metformin and empagliflozin were found to be 2.588 min and 3.679 min and percentage relative standard deviation (RSD) of the metformin and empagliflozin was found to be 0.59 and 1.2, respectively. Percentage recovery was in the range of 100.01–100.65% for metformin and empagliflozin, respectively.Conclusion: A sensitive, rapid, and specific method has been developed for the simultaneous estimation of metformin and empagliflozin using RP-HPLC in tablet dosage form.

scholarly journals ANALYTICAL METHOD DEVELOPMENT AND VALIDATION OF NEW STABILITY-INDICATING REVERSE-PHASE HIGH-PERFORMANCE LIQUID CHROMATOGRAPHY METHOD FOR SIMULTANEOUS ESTIMATION OF METFORMIN HYDROCHLORIDE AND EMPAGLIFLOZIN IN TABLET DOSAGE FORM

2019 ◽  
Vol 12 (1) ◽  
pp. 241
Author(s):  
Geetha Susmita A ◽  
Rajitha G ◽  
Ramya Yadav Y ◽  
Uma P
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
High Performance ◽  
Dosage Form ◽  
Simultaneous Estimation ◽  
Reverse Phase ◽  
Stability Indicating ◽  
Rp Hplc ◽  
Relative Standard ◽  
Tablet Dosage

Objective: The objective of this study was to develop and validate a stability-indicating reverse-phase high-performance liquid chromatography (RP-HPLC) method for the simultaneous estimation of the metformin and empagliflozin in tablet dosage forms.Methods: The chromatographic conditions were optimized and it was run through Std. BDS (250 mm × 4.6 mm, 5 m) column with mobile phase consisting of 0.1% orthophosphoric acid buffer: acetonitrile in the ratio of 50:50. The flow rate was 1 ml/min and optimized wavelength was 210 nm. Temperature was maintained at 30°C.Results: The retention times of metformin and empagliflozin were found to be 2.588 min and 3.679 min and percentage relative standard deviation (RSD) of the metformin and empagliflozin was found to be 0.59 and 1.2, respectively. Percentage recovery was in the range of 100.01–100.65% for metformin and empagliflozin, respectively.Conclusion: A sensitive, rapid, and specific method has been developed for the simultaneous estimation of metformin and empagliflozin using RP-HPLC in tablet dosage form.

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