scholarly journals A Quantitative, Sensitive and Rapid Validated Analytical RP-HPLC Method for the Estimation of Dapagliflozin in Bulk and Pharmaceutical Dosage Formulations

2020 ◽  
Vol 11 (2) ◽  
pp. 2543-2548
Author(s):  
Gouru Santhosh Reddy ◽  
Animesh Bera ◽  
Madhurima Basak ◽  
Krishnaveni Nagappan ◽  
Ramalingam Peraman
Keyword(s):  
High Performance ◽  
Limit Of Detection ◽  
Current Method ◽  
Hplc Method ◽  
Uv Detector ◽  
Limit Of Quantification ◽  
Chromatography Method ◽  
Rp Hplc ◽  
Pharmaceutical Industries ◽  
Liquid Chromatography Method

The present study is aimed to develop a linear, precise, and accurate RP-HPLC (Reverse Phase High-Performance Liquid Chromatography) method for the determination of dapagliflozin in the formulation. The method was accomplished on a C18 column (250×4.6mm; 5µm), & Samples were eluted using acetonitrile: water (40:60%v/v) delivered at a flow rate of 1.0ml/min with a chromatographic run time of 10 min. The eluents were observed utilizing a UV detector with a wavelength set at 277nm. The method that was developed resulted in the retention of dapagliflozin at 7.029minutes. Dapagliflozin through current method has shown linearity (r2 > 0.999) over the concentration range of 1-16 µg/ml. The percentage recovery was observed to be within the limits of 98-102%, demonstrating the accuracy of the method. Limit of detection (LOD) and limit of quantification (LOQ) were qualified at 0.049µg/ml and 0.1485µg/ml, respectively. A Linear, precise, accurate, simple, and rapid RP-HPLC method has been developed and validated for the evaluation of dapagliflozin in bulk drug and tablet dosage forms (5mg &10mg) according to ICH Q2(R1) rules. Additionally, the proposed method could be of use in quality control tests of dapagliflozin in pharmaceutical industries.

HPLC DETERMINATION OF N-METHYLETHANOLAMINE IN DIPHENHYDRAMINE HYDROCHLORIDE DRUG SUBSTANCE BY PRE-COLUMN DERIVATIZATION

INDIAN DRUGS ◽  
2018 ◽  
Vol 55 (10) ◽  
pp. 56-62
Author(s):  
A Anerao ◽  
◽  
V. Dighe ◽  
A Gupta ◽  
C. Patil ◽  
...  
Keyword(s):  
High Performance ◽  
Limit Of Detection ◽  
Active Pharmaceutical Ingredient ◽  
Hplc Method ◽  
Uv Detector ◽  
Limit Of Quantification ◽  
Chromatography Method ◽  
Diphenhydramine Hydrochloride ◽  
Liquid Chromatography Method

N-Methylethanolamine is the side chain of the drug diphenhydramine hydrochloride. A sensitive high performance liquid chromatography method with pre-column derivatization was developed and validated for the determination of N-methylethanolamine impurity in diphenhydramine hydrochloride active pharmaceutical ingredient. HPLC method on column Cosmosil MS-II, C-18, 250 mm X 4.6 mm, particle size 5 μm with UV detector was used. The proposed method is specific, linear, accurate, rugged and precise. The calibration curves showed good linearity over the concentration range of 0.03 mg/g to 1.5 mg/g and the correlation coefficient was 0.999. Method had very low limit of detection (LOD) and limit of quantification (LOQ) as 0.01 mg/g and 0.03 mg/g, respectively, of the analyte. Accuracy was observed within 94.4% to 96.2%.

scholarly journals Simultaneous Estimation and Validation of Atorvastatin Calcium and Aspirin in Combined Capsule Dosage Form by RP HPLC Method

2012 ◽  
Vol 9 (3) ◽  
pp. 1449-1456
Author(s):  
B. V. Suma ◽  
K. Kannan ◽  
V. Madhavan ◽  
Chandini R. Nayar
Keyword(s):  
Limit Of Detection ◽  
Hplc Method ◽  
Simultaneous Estimation ◽  
Uv Detector ◽  
Limit Of Quantification ◽  
Chromatography Method ◽  
Atorvastatin Calcium ◽  
Ich Guidelines ◽  
Phase Liquid ◽  
Liquid Chromatography Method

A new simple, specific, precise and accurate revere phase liquid chromatography method has been developed for estimation of atorvastatin calcium (AST) and ASPIRIN (ASP) simultaneously in a combined capsule dosage forms. The chromatographic separation was achieved on a 5 – micron C 18 column (250x 4.6mm) using a mobile phase consisting of a mixture of Acetonitrile: Ammonium Acetate buffer 0.02M (68:32) pH 4.5. The flow rate was maintained at 0.8 ml/min. The detection of the constituents was done using UV detector at 245 nm for AST and ASP. The retention time of AST and ASP were found be 4.5915 ± 0.0031 min and 3.282 ±0.0024 min respectively. The developed method was validated for accuracy, linearity, precision, limit of detection (LOD) and limit of quantification (LOQ) and robustness as per the ICH guidelines.

scholarly journals Research Article on Development and Validation of RP-HPLC Method for Estimation of Canagliflozin

2019 ◽  
Vol 11 (02) ◽  
pp. 85-92
Author(s):  
Gudipally. Mounika ◽  
K. Bhavya Sri ◽  
R. Swethasri ◽  
M. Sumakanth
Keyword(s):  
Retention Time ◽  
High Performance ◽  
Limit Of Detection ◽  
Hplc Method ◽  
Limit Of Quantification ◽  
Chromatography Method ◽  
Pharmaceutical Dosage Form ◽  
Validation Parameters ◽  
Liquid Chromatography Method ◽  
Development And Validation

To develop an accurate, precise, specific high performance liquid chromatography method for quantification of Canagliflozin in bulk and dosage forms. A C18 column (250mm X 4.6mm; 5μm phenomenex) was used with mobile phase containing Acetonitrile-0.1% sodium acetate buffer (pH-4.6), (20:80) in isocratic mode. The flow rate maintained was 1.0ml/min and the U.V detector was operated at 291nm. The retention time of Canagliflozin was 3.307min and showed a good linearity in concentration range of 2-14μg/ml with correlation coefficient of 0.999. The average percent recovery was found to be 99.98%. The developed method follows validation parameters such as system suitability, linearity, precision, accuracy, limit of detection and limit of quantification and robustness as per ICH guidelinesQ2(R1). The proposed method was found to provide faster retention time with sharp resolution with linearity at a lowest concentration as compared to previous methods and this method is validated as per International conference on harmonization guidelines and successfully applied for bulk and pharmaceutical dosage form.

RAPID HIGH PERFORMANCE LIQUID CHROMATOGRAPHY METHOD FOR THE DETERMINATION OF RALTEGRAVIR IN HUMAN SALIVA

INDIAN DRUGS ◽  
2019 ◽  
Vol 56 (09) ◽  
pp. 68-73
Author(s):  
K Vijaya Sri ◽  
M. Shiva Kumar ◽  
M. A. Madhuri ◽  
Suresha K. ◽  
Keyword(s):  
High Performance ◽  
Limit Of Detection ◽  
High Performance Liquid Chromatographic ◽  
Human Saliva ◽  
Hplc Method ◽  
Limit Of Quantification ◽  
Chromatography Method ◽  
Liquid Chromatography Method ◽  
Liquid Chromatographic

In this study, a high-performance liquid chromatographic method (HPLC) was developed, validated and applied for the determination of raltegravir in biological sample like saliva. Liquid- liquid extraction was performed for isolation of the drug and elimination of saliva interferences. Samples of saliva was extracted with 50µL of ortho phosphoric acid and 3ml of methanol was added and spiked with raltegravir. The chromatographic separation was performed on Agilent Eclipse C18 (100 mm × 4.6 mm, 3.5µm) column, by using 80:20 v/v acetonitrile: water as a mobile phase under isocratic conditions at a flow rate of 1.0 mL/min for UV detection at 240 nm. Retention time of raltegravir was found to be 1.030 min. Linearity was found to be in the range of 25-1000 ng/mL with regression equation y = 13864x + 40495 and correlation coefficient 0.999. The low % RSD value indicates the method is accurate and precise. The limit of detection (LOD) and limit of quantification (LOQ) were found to be 0.76 and 2.28 ng/mL, respectively. It can be concluded that this validated HPLC method is easy, precise, accurate, sensitive and selective for determination of raltegravir in saliva.

scholarly journals Development and validation of novel HPLC method for the estimation of Rutin in crude hydromethanolic leaf extract of Prosopis cineraria

2018 ◽  
Vol 8 (6) ◽  
pp. 68-73
Author(s):  
Ram Singh Bishnoi ◽  
Manish Kumar ◽  
Ajay Kumar Shukla ◽  
C.P. Jain
Keyword(s):  
Mobile Phase ◽  
High Performance ◽  
Limit Of Detection ◽  
Hplc Method ◽  
Detector Response ◽  
Limit Of Quantification ◽  
Chromatography Method ◽  
Prosopis Cineraria ◽  
Liquid Chromatography Method ◽  
Development And Validation

A simple, specific, accurate and precise high performance liquid chromatography method has developed for the estimation of rutin in Prosopis cineraria. The chromatographic separation was achieved by using C18 column, 150 x 4.6mm i.d., 5µ bonded phase octadecylsilane (Thermo Labs Hypersil). Mobile phase was composed of 80 parts of methanol & 20 parts of 0.05% formic acid. The pH of the mobile phase was 3.2.The retention time of rutin was found 5.7 min with 1 mL/min flow rate at ambient temperature. The estimation was performed on PDA detector at 281 nm. In this study, an excellent linearity was obtained with r2 0.999. Besides, the chromatographic peak was found sharp & symmetric. The proposed method was validated in terms of the analytical parameters such as accuracy, linearity, precision, robustness, limit of detection (LOD), limit of quantification (LOQ) were determined based on the International Conference on Harmonization (ICH) guidelines. The detector response was linear in the range of 2-10 µg/mL. The proposed method was successfully applied for the estimation of the constituents in crude extract of Prosopis cineraria. This study established a quantitative method for the determination of rutin from Prosopis cineraria.  Keywords: Prosopis cineraria, HPLC, Validation, Rutin.

scholarly journals A NEW VALIDATED STABILITY-INDICATING DIRECT HIGH-PERFORMANCE LIQUID CHROMATOGRAPHY METHOD FOR THE DETERMINATION OF ROSIGLITAZONE ENANTIOMERS IN THE PRESENCE OF ITS DEGRADATION PRODUCTS

2019 ◽  
pp. 64-67
Author(s):  
BYRAN GOWRAMMA ◽  
SUBRAMANIYAN NAIYANAR MEYYANATHAN ◽  
BASAWAN BABU ◽  
NAGAPPAN KRISHNAVENI
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
High Performance ◽  
Limit Of Detection ◽  
Degradation Products ◽  
Complete Separation ◽  
Uv Detector ◽  
Limit Of Quantification ◽  
Chromatography Method ◽  
Liquid Chromatography Method

Objective: In the present study, an isocratic chiral reverse-phase high-performance liquid chromatography method was developed and the resolution of the drug and complete separation from its degradation products were successfully achieved. Methods: An isocratic method developed with a Phenomenex Lux 5 μ Cellulose 1 (150 mm×4.6 mm i.d., 5 μ) using UV detector at wavelength of 220 nm, with a mobile phase consisting of methanol:0.1% diethylamine (60:40% v/v) and a flow rate of 1 ml/min. The drug was subjected to alkaline, acidic, neutral, oxidative, and photolytic to apply stress conditions. The stressed samples were analyzed by the proposed method. Results: The described method was linear over the range of 3–7 μg/ml for R-enantiomer and 9–21 μg/ml of S-enantiomer, respectively. The limit of detection and limit of quantification of R and S enantiomers were found to be 0.56 μg/ml and 0.18 μg/ml, respectively. Conclusion: The method provides good sensitivity and excellent precision and reproducibility. The developed method can be applied in the quality control of drug products.

scholarly journals NOVEL RP-HPLC METHOD DEVELOPMENT AND VALIDATION FOR ESTIMATION OF TELMISARTAN AND NEBIVOLOL HCL IN PHARMACEUTICAL DOSAGE FORM

2018 ◽  
Vol 11 (9) ◽  
pp. 431 ◽  
Author(s):  
Heena Ar Shaikh ◽  
Vandana Jain
Keyword(s):  
High Performance ◽  
Dosage Form ◽  
Method Development ◽  
Limit Of Detection ◽  
Hplc Method ◽  
Limit Of Quantification ◽  
Pharmaceutical Dosage Form ◽  
Rp Hplc ◽  
Validation Parameters ◽  
Hplc Method Development

Objective: A simple, accurate, precise, robust reverse phase high performance liquid chromatography (RP-HPLC) method was developed for the estimation of telmisartan and nebivolol hydrochloride (HCl) simultaneously in its combined dosage form.Methods: The compounds were well resolved in an isocratic method using the mobile phase composition of acetonitrile: Buffer (potassium dihydrogen orthophosphate pH adjusted 3.1 with orthophosphoric acid) in a ratio of 40:60 v/v at a flow rate of 1.2 ml/min using C18 Shim-pack (150 mm × 4.6 mm, 5 μ) column. The detection was carried out at 280 nm.Results: The retention time of telmisartan and nebivolol HCl was 4.8 min and 6.5 min, respectively. The developed method was validated by evaluating various validation parameters such as linearity, precision, accuracy, robustness, specificity, limit of detection, and limit of quantification according to the international council for harmonization guidelines. The standard calibration curve was obtained in the concentration range of 24–56 μg/ml for telmisartan and 3–7 μg/ml for nebivolol HCl. The overall average % recovery was found out to be 100.35 for telmisartan and 98.84 for nebivolol HCl.Conclusion: Statistical analysis of the data showed that the method is reproducible and selective for the estimation of telmisartan and nebivolol HCl. The proposed method could be used for analysis of telmisartan and nebivolol HCl in their dosage form.

scholarly journals Quantitative Estimation of Sorafenib Tosylate Its Pure Form and in Its Tablet Formulation by RP-HPLC Method

2013 ◽  
Vol 2013 ◽  
pp. 1-3 ◽  
Author(s):  
R. Kalaichelvi ◽  
E. Jayachandran
Keyword(s):  
High Performance ◽  
Quantitative Estimation ◽  
Hplc Method ◽  
Pure Form ◽  
Mobile Phase Composition ◽  
Chromatography Method ◽  
Rp Hplc ◽  
Liquid Chromatography Method ◽  
Isocratic Mode

A simple, accurate, specific reverse-phase, high-performance liquid chromatography method has been developed for the determination of sorafenib tosylate in its pure form and its tablets. In this method, sorafenib tosylate was eluted by isocratic mode using a Phenomenex Luna C18 column by a mobile phase composition of acetonitrile and water in the ratio of 82.5 : 17.5, v/v. The flow rate was 1.5 mL/min. The eluted drug was monitored at 265 nm and the method was found to be linear from 5 to 80 μg/mL. The method was validated by linearity, precision, accuracy, LOD, and LOQ. The accuracy report denotes that there is not any interference of additives used in the formulation.

scholarly journals Determination of Formaldehyde by HPLC with Stable Precolumn Derivatization in Egyptian Dairy Products

2018 ◽  
Vol 2018 ◽  
pp. 1-5 ◽  
Author(s):  
Ahmed Salem Sebaei ◽  
Ahmed M. Gomaa ◽  
A. A. El-Zwahry ◽  
E. A. Emara
Keyword(s):  
Dairy Products ◽  
High Performance ◽  
Limit Of Detection ◽  
Precolumn Derivatization ◽  
Limit Of Quantification ◽  
Chromatography Method ◽  
Derivatizing Agent ◽  
Array Detection ◽  
Liquid Chromatography Method

Formaldehyde is one of the most dangerous chemical compounds affecting the human health; exposure to it from food may occur naturally or by intentional addition. In this study a high performance liquid chromatography method for determination of formaldehyde in dairy products was described. The dairy samples were reacted and extracted with a warmed organic solvent in the presence of derivatizing agent 2,4-dinitrophenylhydrazine (DNPH) and formaldehyde; the mixture was centrifuged and followed by diode array detection. The method is validated and gives average recovery of formaldehyde at the three different levels 0.1, 5.0, and 10.0 mg/kg varied between 89% and 96%. The method is linear from the limit of quantification 0.1 mg/kg up to 10 mg/kg levels. This method is intended for formaldehyde analyses in dairy products simply with stable derivatization, minimum residue loss, excellent recovery, and accurate results with a sensitive limit of detection 0.01 mg/kg. 90 dairy samples from milk, cheese, and yogurt were investigated from seven Egyptian governorates and all samples were free from formaldehyde.

scholarly journals SIMPLE ANALYTICAL METHOD FOR THE SIMULTANEOUS ESTIMATION OF HYDROCHLOROTHIAZIDE AND CANDESARTAN BY RP-HPLC

2017 ◽  
Vol 9 (6) ◽  
pp. 34
Author(s):  
Madhavi K. ◽  
Navamani M. ◽  
Prasanthi C.
Keyword(s):  
High Performance ◽  
Limit Of Detection ◽  
Quantitative Estimation ◽  
High Performance Liquid Chromatographic ◽  
Hplc Method ◽  
Simultaneous Estimation ◽  
Pharmaceutical Dosage Form ◽  
Rp Hplc ◽  
Limit Of Quantitation ◽  
Pharmaceutical Industries

Objective: To develop a simple, rapid, economic, accurate and precise reverse phase-high performance liquid chromatographic (RP-HPLC) method for the determination of hydrochlorothiazide and candesartan in the pharmaceutical dosage form and to validate as per international conference on harmonization (ICH) guidelines.Methods: The chromatographic separation was performed on Silanol BDS C18 column (250 x 4.6 mm, 5 μm), a mobile phase consisting of water (pH adjusted to 2.8 with orthophosphoric acid): acetonitrile (30:70 % v/v), with a flow rate 1 ml/min and the detection wavelength of 210 nm using photodiode array (PDA) detector.Results: The developed method resulted in elution of hydrochlorothiazide at 2.28 min and candesartan at 4.28 min. The calibration curves were linear (r2=0.999) in the concentration range of 6.25-18.75 μg/ml and 8-24 μg/ml for hydrochlorothiazide and candesartan respectively. The percentage recoveries were found to be 99.78-100.39 for hydrochlorothiazide and 99.87-100.64 for candesartan. The limit of detection (LOD) was found to be 0.410 μg/ml and 0.699 μg/ml for hydrochlorothiazide and candesartan respectively. The limit of quantitation (LOQ) was found to be 1.367 μg/ml and 2.330 μg/ml for hydrochlorothiazide and candesartan respectively.Conclusion: A simple, economic, accurate, precise, linear and rapid RP-HPLC method was developed for simultaneous quantitative estimation of hydrochlorothiazide and candesartan in bulk and pharmaceutical formulation and the method was validated as per ICH guidelines. Hence, the method holds good for the routine analysis of hydrochlorothiazide and candesartan in various pharmaceutical industries as well as in academics.

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