scholarly journals Characterization of Impurities in Acarbose Hydrate by using LCMS/MS and NMR

2020 ◽  
Vol 11 (4) ◽  
pp. 8124-8129
Author(s):  
Maruthi R ◽  
Chandan R S ◽  
Anand Kumar Tengli
Keyword(s):  
Dwell Time ◽  
Hplc Method ◽  
Type Ii ◽  
Reverse Phase ◽  
Type Analysis ◽  
Diabetes Mellitus Type Ii ◽  
Injection Volume ◽  
Rp Hplc ◽  
Bulk Drug

An accurate and lively LC-MS/MS and NMR analytical methods have been developed for the recognition and characterization of key impurities in Acarbose. Acarbose is a diabetic medication used to treat Diabetes mellitus Type II and prediabetes in certain countries. Three unknown impurities were detected in Acarbose hydrate bulk drug substance using RP-HPLC method at RT 17.65 min, 18.4 min and 25.85 min. Such impurities have been separated by HPLC and are further characterized by the use of techniques LC-MS / MS and NMR. The C18 reverse phase column and Methanol and Ammonium Type analysis (80:20) have been conducted for the purpose of analysis. With an injection volume of 10 μL, the flow rate was maintained at 0,5mL / min. With binary gradient program, the separations were achieved and the column was kept at ambient temperature. The MS conditions adopted for this analysis with a scan range of m/z = 50 to 500 with a dwell time of 3 seconds. NMR was carried out using DMSO as solvent. Based on spectral data, the impurities have been characterized as IMP B, IMP D and IMP E.

scholarly journals A A RAPID AND SENSITIVE RP-HPLC METHOD FOR THE QUANTITATIVE ANALYSIS OF EMPAGLIFLOZIN IN BULK AND PHARMACEUTICAL DOSAGE FORM

2019 ◽  
pp. 60-65
Author(s):  
MADHURIMA BASAK ◽  
Santhosh Reddy Gouru ◽  
Animesh Bera ◽  
Krishna veni Nagappan
Keyword(s):  
Quantitative Analysis ◽  
High Performance ◽  
Dosage Form ◽  
Limit Of Detection ◽  
Hplc Method ◽  
Reverse Phase ◽  
Pharmaceutical Dosage Form ◽  
Rp Hplc ◽  
Limit Of Quantitation ◽  
Bulk Drug

Objective: The present study aims at developing an accurate precise, rapid and sensitive Reverse Phase High-Performance Liquid Chromatography (RP-HPLC) method for assessing Empagliflozin in bulk drug and in the pharmaceutical dosage form. Methods: The proposed method employs a Reverse Phase Shim Pack C18 column (250 mm × 4.6 mm id; 5 µm) using a mobile phase comprising of acetonitrile and water in the ratio of 60:40 v/v flushed at a flow rate of 1 ml/min. The eluents were monitored at 223 nm. Results: Empagliflozin was eluted at a retention time of 5.417 min and established a co-relation co-efficient (R2>0.999) over a concentration ranging from 0.0495-100µg/ml. Percentage recovery was obtained between 98-102% which indicated that the method is accurate. The Limit of Detection (LOD) and Limit of Quantitation (LOQ) were found at 0.0125µg/ml and 0.0495µg/ml, respectively. Conclusion: An RP-HPLC method which was relatively simple, accurate, rapid and precise was developed and its validation was performed for the quantitative analysis of empagliflozin in bulk and tablet dosage form (10 and 25 mg) in accordance to International Conference of Harmonization (ICH) Q2 (R1) guidelines. The proposed method may aid in routinely analyzing empagliflozin in pharmaceuticals.

scholarly journals A Simple and Validated Reverse Phase HPLC Methodfor the Determination of Rabeprazole inPharmaceutical Dosage Forms

2010 ◽  
Vol 7 (2) ◽  
pp. 569-577 ◽  
Author(s):  
Uma Mahesh Karra ◽  
Sanjeeva Yarkala
Keyword(s):  
High Performance ◽  
Limit Of Detection ◽  
Hplc Method ◽  
Reverse Phase Hplc ◽  
Reverse Phase ◽  
Rp Hplc ◽  
Limit Of Quantitation ◽  
Tablet Formulations ◽  
Bulk Drug

A simple and rapid reverse phase high performance liquid chromatography (RP-HPLC) method was developed and validated for quantitative determination of rabeprazole in bulk drug samples and formulations. Rabeprazole was analyzed by using reverse phase LC-GC column (Inertsil ODS, 4.6 mm x 25 cm, 5 microns), with mobile phase consisting of methanol: water (78:22 v/v). The flow rate was set 1.0 mL/min and analysis was performed at wavelength 288 nm using Photo Diode Array (PDA) detector at ambient temperature. The method was validated and stability studies were conducted under different conditions. The retention time for rabeprazole was around 4.12 minutes. The calibration curves were linear (r≥0.9998) over a concentration range from 20.0 to 80.0 μg/mL. Limit of detection (LOD) and Limit of quantitation (LOQ) were 8 ng/mL and 24 ng/mL respectively. The developed method was successfully applied to estimate the amount of rabeprazole in tablet formulations.

scholarly journals RP-HPLC Method for the Determination of Cinitapride in the Presence of its Degradation Products in Bulk Drug

2010 ◽  
Vol 7 (1) ◽  
pp. 311-319 ◽  
Author(s):  
S. M. N. Roy ◽  
Kiran V. Mangaonkar ◽  
A. Y. Desai ◽  
Santosh M. Yetal
Keyword(s):  
Degradation Products ◽  
Internal Standard ◽  
Hplc Method ◽  
Good Separation ◽  
Reverse Phase Hplc ◽  
Reverse Phase ◽  
Rp Hplc ◽  
Precision And Accuracy ◽  
Bulk Drug

A reverse phase HPLC method is described for the determination of cinitapride hydrogen tartrate in the presence of its degradation products in bulk drug. A drug was subjected to all stress conditions such as reduction, oxidation acidic and alkaline medium. Chromatography was recorded on an Intersil ODS-3 column using mixture of acetonitrile and phosphate buffer, pH adjusted to 6.7 in the ratio (70:30 v/v) as the mobile phase at the rate of 1.0 mL/min with detection at 260 nm. Glimepride was used as internal standard. The retention time of drug cinitapride was 3.8 min and glimepride an internal standard was 2.5 minute. The drug was found to degrade extensively in reduction conditions and mild degradation in the presence of in alkaline, acidic and oxidative but the drug was stable in thermal stress. The method was validated by determining its specificity, linearity, precision and accuracy. The developed method with good separation of all degradation products from drug could be successfully applied for the determination of cinitapride in the presence of its degradation products in the bulk drug. The proposed method is simple, fast, accurate and precise and hence applied for routine quality control of cinitapride in bulk drug. It can be used for analysis of samples during stability testing.

scholarly journals Validated Reverse Phase HPLC Method for the Determination of Irinotecan in Pharmaceutical Dosage Forms

2007 ◽  
Vol 4 (1) ◽  
pp. 128-136 ◽  
Author(s):  
Murali Balaram V. ◽  
VENKATESWARA Rao J. ◽  
Ramakrishnag S. Sankar Ganesh G. ◽  
Balamurali Krishna T.
Keyword(s):  
High Performance ◽  
Limit Of Detection ◽  
Hplc Method ◽  
Reverse Phase Hplc ◽  
Reverse Phase ◽  
Pharmaceutical Dosage Forms ◽  
Rp Hplc ◽  
Limit Of Quantitation ◽  
Bulk Drug

A simple and rapid reverse phase high performance liquid chromatography (RP-HPLC) method was developed and validated for quantitative determination of irinotecan in bulk drug samples and formulations. Irinotecan was analyzed by using reverse phase cyano column (4.6 mmx25 cm, 5 microns), with mobile phase consisting of phosphate buffer: acetonitrile (75:25v/v), pH adjusted to 2.5 with phosphoric acid. The flow rate was set 0.8 mL/min and the analysis was performed at wavelength 225 nm using Photo Diode Array (PDA) detector at ambient temperature. The method was validated and stability studies were conducted under different conditions. The retention time for irinotecan was around 5.82 minutes. The calibration curves were linear (r≥ 0.9998) over a concentration range from 20.0 to 80.0 μg/mL. Limit of detection (LOD) and Limit of quantitation (LOQ) were 8 ng/mL and 24 ng/mL respectively. The developed method was successfully applied to estimate the amount of irinotecan in injection formulations.

Simultaneous Determination of Chloroquine and Pyrimethamine with Cetirizine in an Active Form and Human Serum by RP-HPLC

2021 ◽  
Author(s):  
Hina Shamshad ◽  
Ali Sayqal ◽  
Jahan Zeb ◽  
Agha Zeeshan Mirza
Keyword(s):  
Human Serum ◽  
Simultaneous Determination ◽  
Active Form ◽  
Internal Standard ◽  
Hplc Method ◽  
Serum Samples ◽  
Rp Hplc ◽  
Cetirizine Hydrochloride ◽  
Bulk Drug

Abstract A simple, accurate and precise RP-HPLC method was developed for the simultaneous determination of chloroquine, pyrimethamine and cetirizine hydrochloride concentrations in bulk drug and human serum. The assay was performed using a mobile phase of methanol: water (70:30) at pH of 2.8 ± 0.05 on the Purospher C-18 column with UV detection at 230 nm and rosuvastatin used as an internal standard. The retention times observed for chloroquine, pyrimethamine and cetirizine hydrochloride were 3.5, 2.5 and 5.5 minutes, respectively. The method was found to be specific for the assayed drugs showing a linear response in the concentration range of 1–100 μg mL−1 with coefficients of determination values of (r = 0.999). The method was developed and validated according to ICH guidelines. The method was used to monitor the serum samples and was found to be sensitive for therapeutic purposes, showing the potential to be a useful tool for routine analysis in laboratories.

scholarly journals Development and validation of RP-HPLC method for estimation of brexpiprazole in its bulk and tablet dosage form using Quality by Design approach

2021 ◽  
Vol 7 (1) ◽  
Author(s):  
Amol S. Jagdale ◽  
Nilesh S. Pendbhaje ◽  
Rupali V. Nirmal ◽  
Poonam M. Bachhav ◽  
Dayandeo B. Sumbre
Keyword(s):  
Flow Rate ◽  
High Performance ◽  
Reversed Phase ◽  
Hplc Method ◽  
Control Analysis ◽  
Uv Detector ◽  
Mobile Phase Flow Rate ◽  
Rp Hplc ◽  
Quality By Design Approach ◽  
Bulk Drug

Abstract Background A new, sensitive, suitable, clear, accurate, and robust reversed-phase high-performance liquid chromatography (RP-HPLC) method for the determination of brexpiprazole in bulk drug and tablet formulation was developed and validated in this research. Surface methodology was used to optimize the data, with a three-level Box-Behnken design. Methanol concentration in the mobile phase, flow rate, and pH were chosen as the three variables. The separation was performed using an HPLC method with a UV detector and Openlab EZchrom program, as well as a Water spherisorb C18 column (100 mm × 4.6; 5m). Acetonitrile was pumped at a flow rate of 1.0 mL/min with a 10 mM phosphate buffer balanced to a pH of 2.50.05 by diluted OPA (65:35% v/v) and detected at 216 nm. Result The developed RP-HPLC method yielded a suitable retention time for brexpiprazole of 4.22 min, which was optimized using the Design Expert-12 software. The linearity of the established method was verified with a correlation coefficient (r2) of 0.999 over the concentration range of 5.05–75.75 g/mL. For API and formulation, the percent assay was 99.46% and 100.91%, respectively. The percentage RSD for the method’s precision was found to be less than 2.0%. The percentage recoveries were discovered to be between 99.38 and 101.07%. 0.64 μg/mL and 1.95 μg/mL were found to be the LOD and LOQ, respectively. Conclusion The developed and validated RP-HPLC system takes less time and can be used in the industry for routine quality control/analysis of bulk drug and marketed brexpiprazole products. Graphical abstract

Identification, Characterization, and Quantification of Impurities of Safinamide Mesilate: Process-Related Impurities and Degradation Products

2017 ◽  
Vol 100 (4) ◽  
pp. 1029-1037 ◽  
Author(s):  
Liang Zou ◽  
Lili Sun ◽  
Hui Zhang ◽  
Wenkai Hui ◽  
Qiaogen Zou ◽  
...  
Keyword(s):  
Degradation Products ◽  
Hplc Method ◽  
Formation Mechanisms ◽  
Stability Indicating ◽  
Related Impurities ◽  
Related Substances ◽  
Water Ph ◽  
Bulk Drug ◽  
First Time

Abstract The characterization of process-related impurities and degradation products of safinamide mesilate (SAFM) in bulk drug and a stability-indicating HPLC method for the separation and quantification of all the impurities were investigated. Four process-related impurities (Imp-B, Imp-C, Imp-D, and Imp-E) were found in the SAFM bulk drug. Five degradation products (Imp-A, Imp-C, Imp-D, Imp-E, and Imp-F) were observed in SAFM under oxidative conditions. Imp-C, Imp-D, and Imp-E were also degradation products and process-related impurities. Remarkably, one new compound, identified as (S)-2-[4-(3-fluoro-benzyloxy) benzamido] propanamide (i.e., Imp-D), is being reported here as an impurity for the first time. Furthermore, the structures of the aforementioned impurities were characterized and confirmed via IR, NMR, and MS techniques, and the most probable formation mechanisms of all impurities proposed according to the synthesis route. Optimum separation was achieved on an Inertsil ODS-3 column (250 × 4.6 mm, 5 μm), using 0.1% formic acid in water (pH adjusted to 5.0) and acetonitrile as the mobile phase in gradient mode. The proposed method was found to be stability-indicating, precise, linear, accurate, sensitive, and robust for the quantitation of SAFM and its process-related substances, including its degradation products.

scholarly journals RP-HPLC Determination of Raloxifene in Pharmaceuticl Tablets

2006 ◽  
Vol 3 (1) ◽  
pp. 60-64 ◽  
Author(s):  
P. Venkata Reddy ◽  
B. Sudha Rani ◽  
G. Srinu Babu ◽  
J. V. L. N. Seshagiri Rao
Keyword(s):  
Flow Rate ◽  
Retention Time ◽  
Mobile Phase ◽  
Dosage Forms ◽  
Hplc Method ◽  
Reverse Phase Hplc ◽  
Reverse Phase ◽  
Pharmaceutical Dosage Forms ◽  
Rp Hplc

A reverse phase HPLC method is developed for the determination of Raloxifene in pharmaceutical dosage forms. Chromatography was carried out on an inertsil C18 column using a mixture of acetonitrile and phosphate buffer (30:70 v/v) as the mobile phase at a flow rate of 1 mL/min. Detection was carried out at 290 nm .The retention time of the drug was 10.609 min. The method produced linear responses in the concentration range of 0.5-200 µg/mL of Raloxifene. The method was found to be applicable for determination of the drug in tablets.

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