scholarly journals Reverse Phase Chromatographic Method of Analysis for Assay and Content Uniformity Estimation of Drug Substance Sitagliptin, Metformin and Empagliflozin from Available Marketed Formulation

2021 ◽  
Vol 37 (4) ◽  
pp. 949-961
Author(s):  
Gopal Mohanrao Kadam ◽  
Avinash Laxmanrao Puyad ◽  
Tukaram Mohanrao Kalyankar ◽  
Rajeshwar Vishwanath Kshirsagar
Keyword(s):  
Mobile Phase ◽  
Chromatographic Method ◽  
Drug Substance ◽  
Internal Diameter ◽  
Content Uniformity ◽  
Reverse Phase ◽  
Drug Products ◽  
Accuracy Parameter ◽  
Phase Chemistry ◽  
Intended Use

A new method of analysis with reverse phase chemistry was designed and developed. Validation for method of analysis was performed for its intended use to calculate assay and content uniformity of drug substance sitagliptin, metformin and empagliflozin in the drug products. The method has a run time of 10 minutes on X-bridge C18 column having 250 mm length, 4.6 mm internal diameter and Particle Size of 5µm, by the use of 0.1% Trifluoroacetic acid Buffer 40%: Methanol 40%: Acetonitrile 20% ratio as constituent composition in the proposed mobile phase and chromatography run at wavelength of 224 nm. The retention time of Metformin, Empagliflozin and Sitagliptin, were 3.383, 5.571 and 6.429 minutes, respectively. International Conference on Harmonization guideline was referred for validation. The method showed adequate sensitivity for precision, linearity and accuracy parameter (between the range 25-75μg/mL, 250-750μg/mL and 2.5-7.5μg/mL for sitagliptin, metformin and empagliflozin respectively). The percentage recoveries obtained for sitagliptin, metformin and empagliflozin are in the range of 98.0 – 102.0 %. As results are within the acceptance [1], hence the new developed and proposed method is suitable for quantification of one, two or three component drugs, separately or in combination.

scholarly journals DETERMINATION OF CHROMATOGRAPHIC ASSAY AND VALIDATION OF OFLOXACIN IN BULK AND PHARMACEUTICAL DOSAGE FORM

2018 ◽  
Vol 11 ◽  
Author(s):  
Sumithra M
Keyword(s):  
Mobile Phase ◽  
Dosage Form ◽  
Chromatographic Method ◽  
Assay Method ◽  
Reverse Phase ◽  
Pharmaceutical Dosage Form ◽  
Ich Guidelines ◽  
Validation Parameters ◽  
The Mean

Objective: The objective of the study is simple, sensitive; eco-friendly reverse phase chromatographic method has been developed and validated for the quantitative determination of ofloxacin in bulk and marketed formulation. Method: The developed method was done using Hypersil silica C18 (250 mm × 4.6 mm, 5 μ particle size) as column and the mobile phase is containing water and methanol in the ratio of (10:90) vol/vol. The mobile phase pass at 1 ml/min flow rate and the eluted solution is measured at 270 nm using a PDA detector. Results: The assay method is linear from the concentration range of 5–30 μg/ml. The corelation coefficient is 0.9998. The mean percentage recovery for the developed method is found to be in the range of 98.4–100.6%. The developed method complies robustness studies. Conclusion: The validation of the developed method was done by as per the ICH guidelines. It obeys the linearity, accuracy, precision, and robustness studies. Validation parameters are within the limitations. The results of the developed process indicated the reverse phase chromatographic method is simple, accurate as well as precise, rapid and eco-friendly method for routine analysis of ofloxacin in bulk and its pharmaceutical dosage form.

REVERSE PHASE HIGH PERFORMANCE LIQUID CHROMATOGRAPHIC METHOD FOR DETERMINATION OF BEXAROTENE IN CAPSULE DOSAGE FORM

INDIAN DRUGS ◽  
2018 ◽  
Vol 55 (05) ◽  
pp. 67-71
Author(s):  
N Dhanvijay ◽  
◽  
Vijaya Kumar Munipalli ◽  
M. Patel ◽  
S. Ghani ◽  
...  
Keyword(s):  
Mobile Phase ◽  
High Performance ◽  
Chromatographic Method ◽  
High Performance Liquid Chromatographic ◽  
Control Analysis ◽  
Capsule Formulation ◽  
Reverse Phase ◽  
Liquid Chromatographic Method ◽  
Liquid Chromatographic

A simple precise and rapid Reverse Phase High Performance Liquid Chromatographic method has been developed for quantitative determination of antineoplastic drug bexarotene and its capsule formulation. In this method Synchronis (C18, 25cm×4.6mm id , 5μ) column with mobile phase consisting of buffer (25mM ammonium acetate w/v solution adjusted to pH 4.0 with diluted acetic acid) and acetonitrile in the ratio of (20: 80 v/v) in an isocratic mode was used. The detection was carried out at 262 nm and 20.0 μL injection volume was selected, with the flow rate of 1.0 mL/min being used. The linearity range of bexarotene shows concentration between 5-200 μg/mL. Retention time of bexarotene was found to be 12.58 minutes. Mobile phase itself 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 bexarotene in its formulation.

Simultaneous assay of Mupirocin and Metronidazole in formulations using Reverse Phase-High Performance Liquid Chromatography

2016 ◽  
Vol 5 (12) ◽  
pp. 5151
Author(s):  
Sivannarayana P.* ◽  
K. Rambabu
Keyword(s):  
Mobile Phase ◽  
High Performance ◽  
Chromatographic Method ◽  
High Performance Liquid Chromatographic ◽  
Pharmacokinetic Studies ◽  
Reverse Phase ◽  
Column Temperature ◽  
Ich Guidelines ◽  
Liquid Chromatographic Method ◽  
Liquid Chromatographic

A new reverse phase-high performance liquid chromatographic method for the assay of mupirocin and metronidazole in formulation has been developed and validated as per ICH guidelines. The present study was carried on Water’s X-bridge C-18 column (4.6 x150mm, 5μ particle size) with mobile phase containing a mixture phosphate buffer (pH 2.5) and acetonitrile in the ratio of 70:30, %v/v at a flow rate of 1.0ml/min with UV detection at 220nm in ambient column temperature. The retention times for mupirocin and metronidazole were found to be 2.153 and 3.157 min respectively with linearity in the concentration range of 20-60μg/mL for mupirocin and 10-30μg/mL for metronidazole respectively. The developed reverse phase-high performance liquid chromatographic method was found to be best suitable for pharmacokinetic studies of these mentioned drugs in formulations.

Liquid Chromatographic Methods for Assay of Carbamazepine, 10,11-Dihydrocarbamazepine, and Related Compounds in Carbamazepine Drug Substance and Tablets

1987 ◽  
Vol 70 (5) ◽  
pp. 836-840
Author(s):  
Terry D Cyr ◽  
Fumiko Matsui ◽  
Roger W Sears ◽  
Norman M Curran ◽  
Edward G Lovering
Keyword(s):  
Acetic Acid ◽  
Mobile Phase ◽  
Chromatographic Method ◽  
Drug Substance ◽  
Raw Material ◽  
Aqueous Acetic Acid ◽  
Diol Column ◽  
Liquid Chromatographic ◽  
Related Compounds

Abstract Liquid chromatographic (LC) methods have been developed for the determination of carbamazepine, the impurity 10,11-dihydrocarbamazepine, and related compounds in carbamazepine drug substance and tablets. The LC methods specify a 5 jxm diol column and a mobile phase of acetonitrile-methanol-0.05% aqueous acetic acid (5 + 5 + 90). Iminodibenzyl and iminostilbene, starting materials for some routes of synthesis, elute late in the LC system; therefore, a thinlayer chromatographic method for their detection at the 0.05% level has been developed. Eight tablet and 13 raw material samples from several sources were examined. The impurities most frequently found were 10,11-dihydrocarbamazepine and a compound identified as 10- bromocarbamazepine at levels up to 1.3 and 0.5%, respectively; minimum detectable amounts were about 0.01 and 0.03%, respectively.

Determination of Aztreonam and L-Arginine Combination in Parenteral Formulations

1988 ◽  
Vol 71 (1) ◽  
pp. 31-33
Author(s):  
Abdel-Aziz M Wahbi ◽  
Mohammad A Abounassif ◽  
El-Rasheed A Gad-Kariem ◽  
Mahmoud E Ibrahim ◽  
Hassan Y Aboul-Enein
Keyword(s):  
Mobile Phase ◽  
Chromatographic Method ◽  
Parenteral Formulation ◽  
Reverse Phase ◽  
Liquid Chromatographic Method ◽  
Relative Standard ◽  
Parenteral Formulations ◽  
Liquid Chromatographic ◽  
Phase Column

Abstract A rapid, sensitive and precise liquid chromatographic method is presented for the determination of aztreonam alone, in the presence of its degradation product, and in a parenteral formulation containing L-arginine. A reverse phase column and 0.2M phosphate buffer (pH 6)-methanol (95 + 5) with mobile phase at a flow rate of 2 mL/min is used. The method is sensitive for the range of 10-50 μg/mL with a relative standard deviation of less than 2%. The method has been applied to a parenteral formulation containing aztreonam and L-arginine. L-Arginine is also determined by a nonaqueous titrimetric method.

Determination of Oxytetracycline in Premixes and Veterinary Products by Liquid Chromatography

1986 ◽  
Vol 69 (1) ◽  
pp. 28-30 ◽  
Author(s):  
Gary S Chappell ◽  
Joel E Houglum ◽  
Wesley N Kelley
Keyword(s):  
Mobile Phase ◽  
Chromatographic Method ◽  
Assay Method ◽  
Microbiological Method ◽  
Reverse Phase ◽  
Elution Time ◽  
Liquid Chromatographic Method ◽  
Veterinary Products ◽  
Liquid Chromatographic

Abstract A liquid chromatographic method for the assay of oxytetracycline in premixes and veterinary products is described. Premix samples are extracted with acidified methanol, diluted with mobile phase, and filtered before chromatography on a C-8, reverse phase .column. The assay method separates oxytetracycline from epioxytetracycline, tetracycline, and chlortetracycline. Total elution time for oxytetracycline is less than 5 min at 1.5 mL/min. Five spiked premix samples each of 2 and 50 g/lb had a coefficient of variation of 3.5 and 4.5% and a mean recovery of 99 and 104%, respectively. The results of premixes and veterinary products assayed by this method compared closely with those of the same samples assayed by the official AOAC microbiological method.

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