scholarly journals Stability-indicating HPLC-PDA assay for simultaneous determination of paracetamol, thiamine and pyridoxal phosphate in tablet formulations

2019 ◽  
Vol 69 (2) ◽  
pp. 249-259 ◽  
Author(s):  
Amir Ali ◽  
Muhammad Makshoof Athar ◽  
Mahmood Ahmed ◽  
Kashif Nadeem ◽  
Ghulam Murtaza ◽  
...  
Keyword(s):  
Simultaneous Determination ◽  
Pyridoxal Phosphate ◽  
Degradation Products ◽  
Ammonium Phosphate ◽  
Pharmaceutical Formulations ◽  
Hplc Method ◽  
Complete Separation ◽  
Coefficient Of Determination ◽  
Tablet Formulations

Abstract With the increased number of multi-drug formulations, there is a need to develop new methods for simultaneous determinations of drugs. A precise, accurate and reliable liquid chromatographic method was developed for simultaneous determination of paracetamol, thiamine, and pyridoxal phosphate in pharmaceutical formulations. Separation of analytes was carried out with an Agilent Poroshell C18 column. A mixture of ammonium phosphate buffer (pH = 3.0), acetonitrile and methanol in the ratio of 86:7:7 (V/V/V) was used as the mobile phase pumped at a flow rate of 1.8 mL min−1. Detection of all three components, impurities and degradation products was performed at the selected wavelength of 270 nm. The developed method was validated in terms of linearity, specificity, precision, accuracy, LOD and LOQ as per ICH guidelines. Linearity of the developed method was found in the range 17.5–30 µg mL−1 for thiamine, 35–60 µg mL−1 for pyridoxal phosphate and 87.5–150 µg mL−1 for paracetamol. The coefficient of determination was ≥ 0.9981 for all three analytes. The proposed HPLC method was found to be simple and reliable for the routine simultaneous analysis of paracetamol, thiamine and pyridoxal phosphate in tablet formulations. Complete separation of analytes in the presence of degradation products indicated selectivity of the method.

scholarly journals Stability-indicating RP-HPLC assay for simultaneous determination of chlorpheniramine maleate and prednisolone in veterinary injection

2020 ◽  
Vol 32 (2) ◽  
pp. 122-127
Author(s):  
Amir Ali ◽  
Umar Farooq ◽  
Mahmood Ahmed ◽  
Muhammad Makshoof Athar ◽  
M. Salman ◽  
...  
Keyword(s):  
Simultaneous Determination ◽  
High Performance ◽  
Degradation Products ◽  
Hplc Method ◽  
Complete Separation ◽  
Calibration Graph ◽  
Coefficient Of Determination ◽  
Prednisolone Acetate ◽  
Chlorpheniramine Maleate

The present work described a simple, rapid, sensitive, accurate, and precise method for simultaneous determination of chlorpheniramine maleate (CHRM) and prednisolone acetate (PRED) in injection samples by high-performance liquid chromatography (HPLC) coupled with UV–Vis detection. Chromatographic separation was accomplished, employing isocratic mode and a mobile phase comprised of acetonitrile and a phosphate buffer (50:50, v/v, 30 °C), adjusted to pH 3.0. The flow rate used was 1.0 mL/min on a Thermo Hypersil ODS C18 column (5 μm, 4.6 × 250 mm), and the injection volume of sample was 20 μL. Analysis of CHRM and PRED was performed at a wavelength of 254 nm. The runtime for analysis was 12.5 min, and the retention times of CHRM and PRED were found to be 2.81 and 5.07 min, respectively. The calibration graph showed linearity over the concentration range 10–70 μg/mL for CHRM and 20–140 μg/mL for PRED with a coefficient of determination (R2) ≥0.9986. Repeatability and reproducibility (expressed as % RSD) were lower than 1.72 and 1.47%, respectively. The proposed HPLC method was demonstrated to be simple and rapid for the determination of CHRM and PRED in injection formulation, providing recoveries between 101.6–102.3%, whereas complete separation of degradation products, from analyte under investigation, provided the specificity of the proposed HPLC method.

scholarly journals Stability-indicating RP-HPLC method for simultaneous determination of metformin hydrochloride and vildagliptin in tablet and biological samples

2020 ◽  
Vol 32 (1) ◽  
pp. 39-43
Author(s):  
Abdul Shakoor ◽  
Mahmood Ahmed ◽  
Rabia Ikram ◽  
Sajad Hussain ◽  
Arifa Tahir ◽  
...  
Keyword(s):  
Simultaneous Determination ◽  
Biological Samples ◽  
Degradation Products ◽  
Reversed Phase ◽  
Hplc Method ◽  
Coefficient Of Determination ◽  
Metformin Hydrochloride ◽  
Rp Hplc ◽  
Relative Standard

The present work aimed to develop and validate a simple, rapid, sensitive, accurate, and precise method for simultaneous determination of metformin hydrochloride and vildagliptin in tablet and biological samples. Isocratic elution of both the analytes was performed at 35 °C by injecting 20 μL into Thermo Hypersil ODS C18 column (5 μm, 4.6 mm× 250 mm), while the flow rate was set to 0.8 mL/min. The mobile phase comprised of methanol, acetonitrile, and phosphate buffer (5:30:65, v/v, pH 3.5), and wavelength was selected at 212 nm. The overall run time per sample was 7.0 min with a retention time of 3.36 and 5.41 min for metformin hydrochloride and vildagliptin, respectively. The calibration curve was linear from 10–140 μg/mL for metformin and 1–14 μg/mL for vildagliptin with a coefficient of determination (R2) ≤ 0.9919, while repeatability and reproducibility (expressed as relative standard deviation) were lower than 1.13 and 0.97%, respectively. Force degradation studies indicated a complete separation of the analytes in the presence of their degradation products providing a high degree of method specificity. The proposed reversed-phase high-performance liquid chromatography (RP-HPLC) method was demonstrated to be simple and rapid for the determination of metformin hydrochloride and vildagliptin in commercially available tablet and biological samples providing recoveries ranged between 100.13–100.29%.

scholarly journals Photostability study of amlodipine besylate tablets packed in primary packaging

2021 ◽  
Vol 10 (1) ◽  
pp. 20-28
Author(s):  
Ivana Savić-Gajić ◽  
Ivan Savić ◽  
Predrag Sibinović ◽  
Valentina Marinković
Keyword(s):  
Mobile Phase ◽  
Limit Of Detection ◽  
Degradation Products ◽  
Hplc Method ◽  
Coefficient Of Determination ◽  
Amlodipine Besylate ◽  
Limit Of Quantification ◽  
First Order Kinetics ◽  
The Given

In this study, the modified stability-indicating RP-HPLC method was validated for quantitative analysis of amlodipine besylate in the presence of its impurity D (3-ethyl 5-methyl 2-[(2-aminoethoxy)methyl]-4-(2-chlorophenyl)-6-methylpyridine-3,5-dicarboxylate). The method was applied for the determination of an analyte in the tablets and irradiated samples packed in the primary packaging (Alu/PVC/PVDC blister packaging). The efficient chromatographic separation was achieved using a ZORBAX Eclipse XDB-C18 column (4.6×250 mm, 5 mm) with isocratic elution of mobile phase which consisted of acetonitrile:methanol:triethylamine solution (15:35:50, v/v/v) (pH 3.0). The flow rate of the mobile phase was 1 mL min-1, while the detection of amlodipine besylate was carried out at 273 nm. Amlodipine besylate and its impurity D were identified at the retention times of 16.529 min and 2.575 min, respectively. The linearity of the method with the coefficient of determination of 0.999 was confirmed in the concentration range of 10 - 75 µg mL-1 for amlodipine besylate. The limit of detection was 0.2 µg mL-1, while the limit of quantification was 0.66 µg mL-1. After UV and Vis radiation of the tablets packed in the primary packaging, the content of amlodipine besylate was reduced by 22.38% and 19.89%, respectively. The presence of new degradation products was not detected under the given chromatographic conditions. The photodegradation of amlodipine besylate followed pseudo-first-order kinetics. Based on the half-life of amlodipine besylate (38.4 days for UV radiation and 43.3 days for Vis radiation), it was concluded that amlodipine besylate in the tablets has satisfactory photostability after its packing in the Alu/PVC/PVDC blister packaging.

scholarly journals Development of a New HPLC Method for the Simultaneous Determination of Ticarcillin and Clavulanic Acid in Pharmaceutical Formulations

2009 ◽  
Vol 92 (4) ◽  
pp. 1089-1094
Author(s):  
Tai-Li Tsou ◽  
Chiu-Wey Lee ◽  
Hsian-Jenn Wang ◽  
Ya-Chung Cheng ◽  
Yu-Tien Liu ◽  
...  
Keyword(s):  
Clavulanic Acid ◽  
Simultaneous Determination ◽  
Flow Rate ◽  
Ammonium Acetate ◽  
Pharmaceutical Formulations ◽  
Hplc Method ◽  
Low Flow ◽  
Hplc Separation ◽  
Accuracy And Precision

Abstract A new HPLC method has been developed and validated for the simultaneous determination of ticarcillin (TIC) and clavulanic acid (CA) in pharmaceutical formulations. The HPLC separation was achieved on a -cyclodextrin column (Cyclobond I, 250 4.6 mm, 5 mm) with methanol16 mM pH 6.0 ammonium acetate buffer (50 + 50, v/v) mobile phase at a flow rate of 0.8 mL/min. Detection was at 220 nm. Validation of the method was performed by evaluating specificity, robustness, accuracy, and precision. The calibration curves were linear in the range of 1100 g/mL for CA and 2200 g/mL for TIC. The LOQs based on the standard regression lines were 0.42 and 1.42 g/mL for CA and TIC, respectively, and the LOD were 0.14 and 0.47 g/mL, respectively. Total recoveries of synthetic mixtures (CA:TIC = 1:10, 1:15, and 1:30) were 99.25100.99 for CA and 99.54100.82 for TIC. Compared with the U.S. Pharmacopeia method, the proposed method has the advantage of a relatively low flow rate and short analysis time. The proposed method was successfully applied for the simultaneous determination of these two drugs in sterilized H2O and 5 dextrose injection solutions.

scholarly journals Stability-Indicating Validated HPLC Method for Simultaneous Determination of Oral Antidiabetic Drugs from Thiazolidinedione and Sulfonylurea Groups in Combined Dosage Forms

2010 ◽  
Vol 93 (4) ◽  
pp. 1086-1092 ◽  
Author(s):  
Anna Gumieniczek ◽  
Anna Berecka ◽  
ukasz Komsta
Keyword(s):  
Simultaneous Determination ◽  
Mobile Phase ◽  
Uv Light ◽  
Degradation Products ◽  
Dosage Forms ◽  
Hplc Method ◽  
Base Temperature ◽  
Stability Indicating ◽  
Acid And Base

Abstract For type 2 diabetes treatment, combinations of drugs from the thiazolidinedione and sulfonylurea groups are now available in the same tablet or capsule. Therefore, a stability-indicating and validated HPLC method was developed for simultaneous determination of pioglitazone, rosiglitazone, and glipizide in combined dosage forms. The examined drugs were subjected to different conditions such as acid and base, temperature, and UV light, and degradation of pioglitazone and glipizide was observed under thermal and acidic stress. However, selectivity of the presented method for pioglitazone, rosiglitazone, and glipizide assay against their degradation products was confirmed. It was also demonstrated to be robust, resisting small deliberate changes in pH of the buffer, flow rate, and percentage of acetonitrile in the mobile phase. The presented method utilizes a LiChrospher RP18 column (125 4.0 mm), acetonitrile in phosphate buffer at pH 4.3 (40 + 60, v/v) as the mobile phase, and UV detection at 225 nm for pioglitazone/glipizide or 245 nm for rosiglitazone/glipizide. The method was validated with respect to linearity, precision, and accuracy. Finally, the elaborated procedure was applied for the QC of pioglitazone/glipizide and rosiglitazone/glipizide mixtures.

scholarly journals Simultaneous determination of dexamethasone and moxifloxacin in pharmaceutical formulations using stability indicating HPLC method

2017 ◽  
Vol 10 (3) ◽  
pp. 321-328 ◽  
Author(s):  
Syed Naeem Razzaq ◽  
Muhammad Ashfaq ◽  
Islam Ullah Khan ◽  
Irfana Mariam ◽  
Syed Saleem Razzaq ◽  
...  
Keyword(s):  
Simultaneous Determination ◽  
Pharmaceutical Formulations ◽  
Hplc Method ◽  
Stability Indicating

scholarly journals Development and validation of an RP-HPLC method for the simultaneous determination of Escitalopram Oxalate and Clonazepam in bulk and its pharmaceutical formulations

2012 ◽  
Vol 1 (8) ◽  
pp. 193-198 ◽  
Author(s):  
Chusena Narasimharaju Bhimanadhuni ◽  
Devala Rao Garikapati ◽  
Pasupuleti Usha
Keyword(s):  
Simultaneous Determination ◽  
High Performance ◽  
Pharmaceutical Formulations ◽  
Pharmaceutical Journal ◽  
High Performance Liquid Chromatographic ◽  
Hplc Method ◽  
Validation Parameters ◽  
Tablet Dosage ◽  
Liquid Chromatographic

A Simple, efficient and reproducible reverse phase high performance liquid chromatographic method was developed and validated for the Simultaneous determination of Escitalopram oxalate and Clonazepam in combined dosage form. The separation was effected on a Hypersil ODS C18 column (250mm X 4.6mm; 5µ) using a mobile phase mixture of buffer and acetonitrile in a ratio of 50:50 v/v at a flow rate of 1.0ml/min. The detection was made at 240nm. The retention time of Escitalopram oxalate and Clonazepam was found to be 2.840± 0.007min and 4.007±0.006 min. Calibration curve was linear over the concentration range of 20-120µg/ml and 1-6µg/ml for Escitalopram oxalate and Clonazepam. All the analytical validation parameters were determined and found in the limit as per ICH guidelines, which indicates the validity of the method. The developed method is also found to be precise, accurate, specific, robust and rapid for the simultaneous determination of Escitalopram oxalate and Clonazepam in tablet dosage forms.DOI: http://dx.doi.org/10.3329/icpj.v1i8.11249 International Current Pharmaceutical Journal 2012, 1(8): 193-198 

scholarly journals Simultaneous HPLC Determination of Chlordiazepoxide and Mebeverine HCl in the Presence of Their Degradation Products and Impurities

2015 ◽  
Vol 2015 ◽  
pp. 1-9
Author(s):  
Rania N. El-Shaheny ◽  
Fathalla F. Belal
Keyword(s):  
Simultaneous Determination ◽  
Degradation Product ◽  
Mobile Phase ◽  
Degradation Products ◽  
Potassium Dihydrogen Phosphate ◽  
Hplc Method ◽  
Dihydrogen Phosphate ◽  
Ir Studies ◽  
Validation Procedure

A simple, rapid, and sensitive RP-HPLC method was developed and validated for the simultaneous determination of chlordiazepoxide (CDO) and mebeverine HCl (MBV) in the presence of CDO impurity (2-amino-5-chlorobenzophenone, ACB) and MBV degradation product (veratric acid, VER). Separation was achieved within 9 min on a BDS Hypersil phenyl column (4.5 mm × 250 mm, 5 µm particle size) using a mobile phase consisting of acetonitrile: 0.1 M potassium dihydrogen phosphate: triethylamine (35 : 65 : 0.2, v/v/v) in an isocratic mode at a flow rate of 1 mL/min. The pH of the mobile phase was adjusted to 4.5 with orthophosphoric acid and UV detection was set at 260 nm. A complete validation procedure was conducted. The proposed method exhibited excellent linearity over the concentration ranges of 1.0–100.0, 10.0–200.0, 2.0–40.0, and 2.0–40.0 µg/mL for CDO, MBV, VER, and ACB, respectively. The proposed method was applied for the simultaneous determination of CDO and MBV in their coformulated tablets with mean percentage recoveries of 99.75 ± 0.62 and 98.61 ± 0.38, respectively. The results of the proposed method were favorably compared with those of a comparison HPLC method using Studentt-test and the variance ratioF-test. The chemical structure of MBV degradation product was ascertained by mass spectrometry and IR studies.

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