scholarly journals A NOVEL STABILITY-INDICATING REVERSE PHASE LIQUID CHROMATOGRAPHIC METHOD FOR THE SIMULTANEOUS ESTIMATION OF METFORMIN AND TENELIGLIPTIN IN PURE AND PHARMACEUTICAL FORMULATIONS

Author(s):  
A. Swetha ◽  
B. Ramya Kuber

Objective: The present method was proposed to develop a simple, sensitive, rapid, accurate and stability-indicating reverse phase liquid chromatographic method for the simultaneous estimation of metformin and teneligliptin in pure and pharmaceutical formulations. Methods: The chromatographic separation was done on Discovery [250 mm X 4.6 mm: 5 μm is particle size] using a mobile phase composed of 0.1% orthophosphoric acid buffer: acetonitrile [65:35, v/v], the flow rate is 1 ml/min and the detection was carried out at 260 nm.Results: The retention time of metformin and teneligliptin were found to be 2.517 min and 3.687 min, respectively. Stability indicating studies were conducting under the guidelines of an international conference on harmonization [ICH] Q1A R2 and the developed method was validated as per guidelines of ICH Q2 RI. The linearity was found in the range of concentration of 125-750 μg/ml and 5-30 μg/ml for metformin and teneligliptin. The detection of limit and quantification of limit was found to be 0.02 μg/ml and 0.07 μg/ml for metformin and 0.19 μg/ml and 0.56 μg/ml for teneligliptin, respectively.Conclusion: A novel stability-indicating reverse-phase liquid chromatographic method for the simultaneous estimation of metformin and teneligliptin. The proposed method was adopted for the routine estimation of metformin and teneligliptin in bulk and pharmaceutical dosage forms. 

2018 ◽  
Vol 10 (5) ◽  
pp. 274
Author(s):  
A. Swetha ◽  
B. Ramya Kuber

Objective: The present method was proposed to develop a simple, sensitive, rapid, accurate and stability-indicating reverse phase-high performance liquid chromatographic (RP-HPLC) method for the simultaneous estimation of metformin and teneligliptin in pure and pharmaceutical formulations. Methods: The chromatographic separation was done on Discovery [250 mm X 4.6 mm: 5 μm is particle size] using a mobile phase composed of 0.1% orthophosphoric acid buffer: acetonitrile [65:35, v/v], the flow rate is 1 ml/min and the detection was carried out with a photodiode array (PDA) at 260 nm.Results: The retention time of metformin and teneligliptin were found to be 2.517 min and 3.687 min, respectively. Stability indicating studies were conducted under the guidelines of an international conference on harmonization [ICH] Q1A R2 and the developed method was validated as per the guidelines of ICH Q2 R1. The linearity was found in the range of concentration of 125-750 μg/ml and 5-30 μg/ml for metformin and teneligliptin. The lower limit of detection (LOD) and lower limit of quantification (LOQ) was found to be 0.02μg/ml and 0.07 μg/ml for metformin and 0.19 μg/ml and 0.56 μg/ml for teneligliptin, respectively.Conclusion: A novel stability-indicating reverse phase liquid chromatographic method developed for the simultaneous estimation of metformin and teneligliptin. The proposed method was adopted for the routine estimation of metformin and teneligliptin in bulk and pharmaceutical dosage forms.


Author(s):  
SWETHA A ◽  
RAMYA KUBER B

Objective: The objective of the study was to develop a novel, simple, sensitive, accurate, precise, and stability-indicating reverse-phase (RP) liquid chromatographic method for simultaneous estimation of sofosbuvir and daclatasvir in pure and pharmaceutical formulation. Methods: In the present work, chromatographic separation was done using stationary-phase discovery column (250 mm×4.6 mm; 5 μm particle size) and mobile phase consisting of 0.1N potassium dihydrogen orthophosphate buffer:acetonitrile (55:45, v/v), with the flow rate of 1 ml/min, and the detection of column effluents was achieved with photodiode array at 260 nm. Results: The retention time of sofosbuvir and daclatasvir was found to be 2.32 min and 3.06 min, respectively. Stability-indicating studies were conducted according to the guidelines of International Conference on Harmonization (ICH) Q1A R2, and validation of the method was done as per the ICH guidelines Q2R1. The linearity of the method was in the concentration range of 100–600 μg/ml and 15–90 μg/ml for sofosbuvir and daclatasvir, respectively. The correlation coefficients were found to be 0.9996 and 0.9996 for sofosbuvir and daclatasvir, respectively. The limit of detection and limit of quantification were found to be 0.19 μg/ml and 0.59 μg/ml for sofosbuvir and 0.02 μg/ml and 0.05 μg/ml for daclatasvir, respectively. Conclusion: The stability-indicating RP high-performance liquid chromatographic (RP-HPLC) method was novel, simple, precise, accurate, and sensitive for simultaneous estimation of sofosbuvir and daclatasvir in pure and pharmaceutical formulations. Hence, the developed method was adopted for qualitative and quantitative analysis of sofosbuvir and daclatasvir in pure and pharmaceutical formulations.


Author(s):  
MUNI SAI VARAGANTI ◽  
PRASANTHI CHENGALVA ◽  
ARUNA GUNDALA

Objective: A combination of hydrocortisone and tetracycline as topical ophthalmic ointment is used for skin irritations, eye infections, inflammation, skin infections, acne, and rashes. The objective of the current work is to a simple, rapid, accurate, and precise, stability-indicating reverse-phase liquid chromatographic method was developed for the simultaneous estimation of hydrocortisone and tetracycline in bulk and pharmaceutical dosage form. Methods: The separation was carried out in Discovery C18 column (250 × 4.6 mm, 5 μm) using mobile phase ratio of water (pH 2.2 adjusted with orthophosphoric acid):acetonitrile (40:60 v/v) in an isocratic elution mode with a flow rate of 1.0 ml/min at detection wavelength of 244 nm. The injection volume was 10 μl and the column temperature was set at 30°C. Results: The retention time for hydrocortisone and tetracycline was found to be 2.214 ± 0.001 min and 3.497 ± 0.001 min, respectively. Calibration curves were linear (r2=0.999) at a concentration range of 2.5–15 mg/ml for both hydrocortisone and tetracycline. The percentage recoveries were found to be 99.13–99.67% for hydrocortisone and 99.39–99.61% for tetracycline. Relative standard deviation was found to be 0.3% for both the drugs. Limit of detection and limit of quantification values of hydrocortisone and tetracycline were found to be 0.09 μg/ml and 0.27 μg/ml and 0.17 μg/ml and 0.52 μg/ml, respectively. The drugs were subjected to various stress conditions and found no interference of degraded products peak at the retention times of analyte peaks. Conclusion: A rapid and accurate reverse-phase high-performance liquid chromatographic method was developed for simultaneous estimation of hydrocortisone and tetracycline, and the method was validated as per the International Council for Harmonization guidelines. Hence, the developed method can be successfully applied for the simultaneous estimation of hydrocortisone and tetracycline in bulk and ointment formulation.


Author(s):  
Vijaya Jyothi M ◽  
Bhargav E ◽  
Keerthana B ◽  
Varalakshmi Devi K

The combination of Irinotecan Hydrochloride (IRI) and Capecitabine (CAP) is indicated for the treatment of cancer. IRI and CAP were developed by an simultaneous simple reverse phase liquid chromatographic method and were subsequently validated from their APIs. The proposed method was based upon the separation of these two chemical agents using Agilent 1200 series HPLC with Qualisil gold C18 (250 × 4.6 mm, 5µ) column and it was maintained at ambient temperature. The effective chromatogram was obtained using the mobile phase of methanol: water (60:40 (% v/v)) and the pH was adjusted to 3 with orthophosphoric acid at the flow rate of 1.0 ml/min. The column effluents were detected using Photo Diode array detector at wavelength of 340 nm. The proposed reverse phase liquid chromatographic method was validated as per ICH Q2 (R1) guidelines. Based upon the optimized parameters, these drugs were effectively separated and the retention time was found at 4.08 min. for IRI and 7.8 min. for CAP with resolution of 7.6. There is no interference with the impurities or degradation products. The calibration plots were found to be linear over the concentration range of 4-24 µg/ml and 40-240 µg/ml respectively. The LOD and LOQ of IRI were found to be 0.12 µg/ml and 0.373 µg/ml while LOD and LOQ of CAP were found to be 0.254 µg/ml and 0.771 µg/ml respectively. The mean percent recovery of triplicate analysis of IRI and CAP were found to be 100.58% and 100.03% respectively. In conclusion, the developed method can be used in the quality control laboratories for the determination of IRI and CAP in APIs. Keywords: RP-HPLC; Irinotecan Hydrochloride; Capecitabine; Validation


1988 ◽  
Vol 71 (1) ◽  
pp. 53-55 ◽  
Author(s):  
Kenneth M Weaver ◽  
Michael E Neale ◽  
Ann Laneville

Abstract A method was developed for the detection and quantitation of piperine in Piper nigrum. A reverse-phase liquid chromatographic system equipped with a C18 column with detection at 340 nm was used. A rapid 1 h acetone extraction followed by solvent dilution was used to avoid sample cleanup. The detection limit is 3 ng injected piperine, with 97.5-100.5% recovery of added piperine.


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