Development of RP-HPLC Method for Estimation of Valsartan and Hydrochlorothiazide in Tablets

Author(s):  
Cylma Menezes ◽  
Vishal M ◽  
Shyamkumar B ◽  
Reema N

A simple, efficient and reproducible reversed phase high performance liquid chromatographic (RP-HPLC) method was developed and validated for the simultaneous estimation of valsartan and hydrochlorothiazide in bulk and in tablets. A column having 250 x 4.6 mm i.d. (Kromasil C18) in isocratic mode with mobile phase containing 50 mM potassium dihydrogen o-phosphate buffer (triethylamine 0.2%), (pH 3.7 adjusted with o-phosphoric acid): acetonitrile (56:44 v/v) was used. The flow rate was 1.0 ml/min and effluent was monitored at 232 nm.  The retention time of valsartan and hydrochlorothiazide was 10.15 and 3.78 min respectively. All calibration curves showed good linear correlation coefficients within the tested limits (r2 > 0.9995). The linearity dynamic range was found to be 20-150 µg/ml and 5-45 µg/ml for valsartan and hydrochlorothiazide respectively. Percentage recoveries for valsartan and Hydrochlorothiazide were 100.45 % and 98.75 % respectively. All the analytical validation parameters were determined and found in the limit as per the International Conference on Harmonization (ICH) guidelines which indicates the validity of the method. The developed method was found to be accurate, precise and robust for the simultaneous estimation of valsartan and hydrochlorothiazide in bulk and in tablets.

2012 ◽  
Vol 10 (2) ◽  
pp. 67-70
Author(s):  
Abdullah Al Masud ◽  
Mohammad Saydur Rahman ◽  
Towfika Islam ◽  
Saki Sultana ◽  
Moynul Hasan ◽  
...  

A simple, reproducible and efficient reversed phase high performance liquid chromatographic (RPHPLC) method has been developed for the estimation of a recently approved anti allergic drug, amlexanox in oral paste dosage form. The separations were carried out on a Zorbax Eclipse XBD, C18 column (150 x 4.6 mm; 5?m) at a flow rate of 1.50 ml/min. by using mobile phase comprising of mixed buffer (pH adjusted to 6.50) and methanol (50:50 v/v). The injection volume was 10 ?l and the peaks were detected at 244 nm. The linear dynamic range found to be in the concentration range of 15-35 ?g/ml and coefficient of correlation was found to be 0.999. The %RSD value was below 2.0 for intra-day and inter-day precision which indicated that the method was highly precise. The LOD (Limit of detection) and LOQ (Limit of quantitation) were found to be 3.8 ng/ml and 12.5 ng/ml, respectively which revealed that the method was highly sensitive. The percentage recovery of amlexanox ranged from 99.31 to 99.75%, indicating the accuracy of the method and absence of interference from the excipients present in the formulation. The proposed method was simple, fast, accurate and reproducible and hence can be applied for routine quality control operations of amlexanox in oral paste dosage form. Key words: Amlexanox, Anti allergic, RP-HPLC, LOD, LOQ. DOI: http://dx.doi.org/10.3329/dujps.v10i2.11782 Dhaka Univ. J. Pharm. Sci. 10(2): 67-70, 2011 (December)


2019 ◽  
Vol 9 (01) ◽  
pp. 83-88
Author(s):  
Pinkal Patel ◽  
Nalini Patel ◽  
Kinjal Parmar

A simple, selective and rapid reversed phase High Performance Liquid Chromatographic (RP-HPLC) method has been developed and validated for the simultaneous analysis Gatifloxacin and flurbiprofen sodium in eye drops. The separation was carried out using a mobile phase consisting ACN: Buffer (pH 3.5) in the ratio of 55:45 v/v. The column used was Phenomenex luna ODS C18 (250mm X 4.6 mm i.d., 5 μm particle size) with flow rate of 1 ml / min using UV detection at 268 nm. The described method was linear over a concentration range of 2-12 μg/ml for both of Gatifloxacin and flurbiprofen sodium. The retention times of Gatifloxacin and flurbiprofen sodium were found to be 3.710 min. and 6.797 min respectively. Method was validated statistically and recovery studies were carried out. The proposed method has been applied successfully to the analysis of cited drugs either in pure form or in pharmaceutical formulations with good accuracy and precision. The method here in described can be employed for quality control and routine analysis of drugs in pharmaceutical formulations.


INDIAN DRUGS ◽  
2019 ◽  
Vol 56 (02) ◽  
pp. 39-46
Author(s):  
Babu D. China ◽  
◽  
C. Madhusudhana Chetty ◽  
Sk. Mastanamma

A simple, accurate, precise and robust reversed phase high performance liquid chromatographic (RP-HPLC) method was developed for the estimation of Ertugliflozin (ETZ) and metformin (MFN) in bulk and in tablet dosage form. The method was carried out by used Waters (5μm, C18 250 x 4.6 mm) column with mobile phase consists of 0.75 mM sodium dihydrogen orthophosphate buffer pH adjusted to 8.5, with NaOH, and acetonitrile in the ratio of 60:40 v/v, a flow rate of 1.5 mL/min and photodiode detection at 263 nm. The method was validated as per ICH guidelines with different parameters, the mean retention times of ertugliflozin and metformin were found to be 3.5& 2.0 min, respectively. The correlation coefficient values of calibration curves were found to be 0.999 for both ETZ and MFN, respectively. The LOD and LOQ for ertugliflozin and metformin were found to be 0.02-0.06 μg/mL and 17.5-58.3 μg/mL respectively.


INDIAN DRUGS ◽  
2015 ◽  
Vol 52 (08) ◽  
pp. 12-16
Author(s):  
S Vidyadhara ◽  
◽  
L. S Reddyvalam ◽  
T. Koduri ◽  
P. K. Borra ◽  
...  

A simple, accurate, precise high-performance liquid chromatographic (HPLC) method has been developed and validated for the simultaneous determination of abacavir sulphate (ABA) and lamivudine (LAM) in combined dosage form. Separation was performed on a C18 column [Agilent ODS UG 5 column, 250 mm x 4.5 mm], with methanol: water (50:50 V/V) isocratic elution using a flow rate of 1mL/min. Good sensitivity was observed with UV detection at 277 nm. After method development, the interference of other active compounds and excipients, repeatability and linearity, were investigated. Retention times of LAM and ABA were found to be 3.3 and 6.3 min, respectively. The method was validated over the range from 2.5-12.5 μg/mL for LAM and 5-25 μg/mL for ABA with correlation coefficients of 0.9997 and 0.9996, respectively. This method was shown to be accurate, robust, selective, linear, and repeatable and can be successfully employed in routine quality control for the simultaneous analysis of ABA and LAM in tablets.


2008 ◽  
Vol 91 (4) ◽  
pp. 739-743 ◽  
Author(s):  
Andréia de Haro Moreno ◽  
Hérida Regina Nunes Salgado

Abstract A rapid, accurate, and sensitive high-performance liquid chromatographic (HPLC) method was developed and validated for the determination of ceftazidime in pharmaceuticals. The method validation parameters yielded good results and included range, linearity, precision, accuracy, specificity, and recovery. The excipients in the commercial powder for injection did not interfere with the assay. Reversed-phase chromatography was used for the HPLC separation on a Waters C18 (WAT 054275; Milford, MA) column with methanolwater (70 + 30, v/v) as the mobile phase pumped isocratically at a flow rate of 1.0 mL/min. The effluent was monitored at 245 nm. The calibration graph for ceftazidime was linear from 50.0 to 300.0 g/mL. The values for interday and intraday precision (relative standard deviation) were <1. The results obtained by the HPLC method were calculated statistically by analysis of variance. We concluded that the HPLC method is satisfactory for the determination of ceftazidime in the raw material and pharmaceuticals.


2008 ◽  
Vol 91 (5) ◽  
pp. 1070-1074 ◽  
Author(s):  
Arun M Prajapati ◽  
Satish A Patel ◽  
Natvarlal J Patel ◽  
Dipti B Patel ◽  
Sejal K Patel

Abstract This research paper describes validated reversed-phase high-performance column liquid chromatographic (RP-HPLC) and first-derivative UV spectrophotometric methods for the estimation of voriconazole (VOR) in oral suspension powder. The RP-HPLC separation was achieved on Phenomenex C18 column (250 4.6 mm id, 5 m particle size) using wateracetonitrile (40 + 60, v/v; pH adjusted to 4.5 0.02 with acetic acid) as the mobile phase at a flow rate of 1.4 mL/min and ambient temperature. Quantification was achieved with photodiode array detection at 255 nm over the concentration range of 0.11 g/mL with mean recovery of 99.49 0.83 for VOR by the RP-HPLC method. Quantification was achieved with UV detection at 266 nm over the concentration range of 820 g/mL with mean recovery of 99.74 0.664 for VOR by the first-derivative UV spectrophotometric method. These methods are simple, precise, and sensitive, and they are applicable for the determination of VOR in oral suspension powder.


2017 ◽  
Vol 15 (2) ◽  
pp. 187-194 ◽  
Author(s):  
Md Shahadat Hossain ◽  
Md Samiul Islam ◽  
Subrata Bhadra ◽  
Abu Shara Shamsur Rouf

Highly nutritious dairy products are ingested regularly by all ages of population. Adulteration of dairy products to enhance the inherent stability and acceptability to common consumers by different harmful and toxic ingredients like formalin, an unpermitted preservative, has been a burning issue in Bangladesh over the last few years. The aim of this paper was to analyze the concentration of formaldehyde in dairy products most commonly sold in Bangladeshi markets by a validated reversed phase high performance liquid chromatographic (RP-HPLC) method to reveal the on-going alarming scenario in a scientific way. After pre-derivatization with 2,4- dinitrophenylhydrazine, formaldehyde was detected at 345 nm using a C18 column with acetonitrile and water (45:55) as mobile phase at a flow rate of 2.0ml/min. The validated method has been applied to 41 marketed dairy products, including pasteurized milk, UHT milk, banana- mango- and chocolate-milk, flavored yoghurt, lassi, buttermilk, and skimmed milk. However, no formaldehyde was detected among the tested dairy products.Dhaka Univ. J. Pharm. Sci. 15(2): 187-194, 2016 (December)


1970 ◽  
Vol 3 (1) ◽  
pp. 49-53 ◽  
Author(s):  
Gaurav Patel ◽  
Sanjay Patel ◽  
Dhamesh Prajapiti ◽  
Rajendra Mehta

A reverse phase high performance liquid chromatographic (RP-HPLC) method has been developed for the simultaneous estimation of Amlodipine Besylate and Hydrochlorothiazide in combine dosage form. Amlodipine Besylate (AML) is a long acting calcium channel blocker and in the treatment of CVS disorder. Hydrochlorothiazide (HCT) is a diuretic and antihypertensive. The mobile phase used was a combination of Water: Methanol (70:30). The detection of the combined dosage form was carried out at 245nm and a flow rate employd was 0.5ml/min. The retention time for Amlodipine Besylate and Hydrochlorothiazide was found to be 6.95 and 2.65 min respectively. Linearity was obtained in the concentration range of 6 to 18μg/ml of Amlodipine Besylate and 6 to 18μg/ml of Hydrochlorothiazide with a correlation coefficient of 0.997 and 0.9974. Detector consists of photodiode array detector; the reversed phase column used was RP-C18 (5 μm size, 250mm, 4.6mm i.d.) at ambient temperature. The developed method was validated according to ICH guidelines and values of accuracy, precision and other statistical analysis were found to be in good accordance with the prescribed values. Thus the proposed method is precise, selective and rapid for simultaneous estimation of Amlodipine Besylate and Hydrochlorothiazide in routine analysis. Key Words: Simultaneous Estimation; Amlodipine Besylate; Hydrochlorothiazide; HPLC. DOI: 10.3329/sjps.v3i1.6798S. J. Pharm. Sci. 3(1): 49-53


2009 ◽  
Vol 63 (6) ◽  
Author(s):  
Hong Yan ◽  
Pei Xu ◽  
Hai Huang ◽  
Juan Qiu

AbstractA pre-column derivatized high-performance liquid chromatographic (HPLC) method with ultraviolet-visible detection was developed to measure the concentrations of spectinomycin in fermentation broth. Derivatization reagents, 2,4-dinitrophenylhydrazine in acetonitrile (5 mg mL−1) and trifluoroacetic acid in acetonitrile (0.8 mol L−1), were added to an aliquot of the fermentation broth, and the mixture was incubated for 60 min at 70°C. The resulting derivative was separated from other compounds by isocratic elution in a reversed-phase column Zorbax SB-C18 (250 mm × 4.6 mm, 5 µm). Mobile phase consisted of acetonitrile, tetrahydrofuran, and water (φ r = 40: 35: 25) and the flow rate was 1.0 mL min−1. The detection wavelength was 415 nm. The standard curve for spectinomycin sulfate was linear with correlation coefficients of 0.9997 in the range of 25 µg mL−1 to 600 µg mL−1. The relative standard deviation values ranged from 0.43 % to 2.18 % depending on the concentration of samples. The average recovery was 101.5 %. The limit of detection was 50 ng mL−1.


2018 ◽  
Vol 8 (6-s) ◽  
pp. 78-82 ◽  
Author(s):  
Vishal Singh Solanki ◽  
RAM SINGH BISHNOI ◽  
Raviraj Baghel ◽  
Deepti Jain

A simple precise and economical reverse phase high performance liquid chromatographic method has been developed and validated for the simultaneous estimation of Cilnidipine (CDP), Atenolol (ATL) and Chlorthalidone (CTD).The chromatographic separation was achieved by using Hypersil- keystone C18 (4.6 x 250mm, 5μm) under isocratic conditions The mobile phase consisted of methanol and triple distilled water (80/20, v/v) having pH 7 with a flow rate of 1.0 mL/min. The eluents were monitored at 225 nm for simultaneous measurement.The selected chromatographic conditions were found to effectively separate CDP (Rt: 3.25 min), ATL (Rt: 5.366 min) and CTD (Rt: 9.025 min) having good resolution. The developed method was validated for linearity, accuracy, precision, LOD, LOQ, robustness and for system suitability parameters as per ICH guidelines. In this study, an excellent linearity was obtained with r2 = 0.999, r² = 0.999, r² = 1, for CDP, ATL and CTD respectively. The developed chromatographic method proved to be simple, precise, accurate, robust and reproducible Thus, this method would be employed for routine simultaneous quantification of CDP, ATL and CTD in bulk form or tablet dosage form.   Keywords: Cilnidipine, Atenolol and Chlorthalidone, RP-HPLC.


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