scholarly journals Development and Validation for the Simultaneous Quantification of Nebivolol Hydrochloride and Hydrochlorothiazide by UV Spectroscopy, RP-HPLC and HPTLC in Tablets

2010 ◽  
Vol 7 (2) ◽  
pp. 341-348 ◽  
Author(s):  
B. Dhandapani ◽  
N. Thirumoorthy ◽  
D. Jose Prakash
Keyword(s):  
Mobile Phase ◽  
Uv Spectroscopy ◽  
Internal Standard ◽  
Simultaneous Equation ◽  
Equation Method ◽  
Ratio Method ◽  
Simultaneous Quantification ◽  
Rp Hplc ◽  
Absorbance Ratio ◽  
Nebivolol Hydrochloride

Simultaneous quantification of nebivolol hydrochloride (NEB-H) and hydrochlorothiazide (HCT) in tablets by UV spectroscopy, RP-HPLC and HPTLC methods were developed. In UV spectrophotometric determination NEB-H and HCT was quantified by simultaneous equation method and absorbance ratio method. In simultaneous equation method absorbance measurements at 282.5 nm (λmaxNEB-H) and 271.5 nm (λmaxHCT), in absorbance ratio method absorbance measurements at 282.5 nm and 275 nm (iso absorptive point) in methanol. In RP-HPLC method, the drugs were resolved using a mobile phase of 30 mM phosphate buffer (K2HPO4), acetonitrile and triethylamine (50:50:0.1 % v/v) with pH 5.5 using orthophosphoric acid on a C18-ODS- Phenomenex (5 μm, 250 mm x 4.6 mm) column in isocratic mode, Atorvastatin (ATR) used as a internal standard. The retention time of HCT, NEB-H and ATR was 3.31, 4.30 and 6.93 min respectively. In the HPTLC method, the chromatograms were developed using a mobile phase of ethyl acetate: methanol: ammonia (8.5:1:0.5 v/v) on precoated plate of silica gel 60 F254and quantified by densitometric absorbance mode at 285 nm. The Rf of HCT and NEB-H were 0.21 and 0.41 respectively. Recovery studies of 98.88-102.41%, percentage relative std deviation of not more than 0.8 and correlation coefficient (linearity range) of 0.9954-0.9999 shows that developed methods were accurate and precise. These methods can be employed for the routine analysis of tablets containing NEB-H and HCT.

SIMULTANEOUS ESTIMATION OF CURCUMIN AND GEFITINIB IN BULK AND TISSUE SAMPLES (PLASMA AND BRAIN HOMOGENATE) BY RP-HPLC: APPLICATION TO A DISTRIBUTION STUDY

INDIAN DRUGS ◽  
2019 ◽  
Vol 56 (07) ◽  
pp. 59-68
Author(s):  
H Mahajan ◽  
S Savale ◽  
P Nerkar ◽  
Keyword(s):  
Flow Rate ◽  
Mobile Phase ◽  
Internal Standard ◽  
Brain Homogenate ◽  
Reversed Phase ◽  
Hplc Method ◽  
Simultaneous Estimation ◽  
Bulk Analysis ◽  
Experimental Conditions ◽  
Rp Hplc

The present study was aimed at developing a Reversed-Phase High-Performance Liquid Chromatography (RP-HPLC) method for simultaneous determination of curcumin (CRM) and gefitinib (GFT) in bulk, plasma and brain homogenate. hydrochlorothiazide was used as an internal standard (IS). A new simple, rapid, selective, precise and accurate RP-HPLC method has been developed. The separation was achieved by using C-18 column (Qualisil BDS C18, 250 mm x 4.6 mm I.D.) coupled with a guard column of silica, mobile phase consisted of acetonitrile: water with 0.1% formic acid (30:70 v/v). The flow rate was 0.2 ml/min and the drug was detected using PDA detector at the wavelength of 242 nm. The experimental conditions, including the diluting solvent, mobile phase composition, column saturation and flow rate, were optimised to provide high-resolution and reproducible peaks. The method was developed and tested for linearity range of 10-60 μg/mL for bulk analysis and 200-800 ng/mL for plasma and brain homogenate. The developed method was validated as per ICH guidelines, in terms of linearity, application of the proposed method to bulk sample, recovery, precision, repeatability, ruggedness, sensitivity (LOD and LOQ) and robustness and stability study (short and long-term stabilities, freeze/thaw stability, post-preparative). The low value of % RSD showed that the method was precise within the acceptance limit of 2%. The developed method was successfully applied for the analysis of the drug in bulk as well as various marketed formulation and drug in plasma and brain distribution studies.

scholarly journals ULTRAVIOLET SPECTROSCOPY AND ITS PHARMACEUTICAL APPLICATIONS- A BRIEF REVIEW

2018 ◽  
Vol 11 (2) ◽  
pp. 59 ◽  
Author(s):  
Dipali M Atole ◽  
Hrishikesh H Rajput
Keyword(s):  
Simultaneous Equation ◽  
Ratio Method ◽  
Isosbestic Point ◽  
Complex Matrix ◽  
Spectrophotometric Methods ◽  
Factor Method ◽  
Absorbance Ratio ◽  
Present Information ◽  
Different Types ◽  
Absorbance Difference

 Rapid and easy analytical methods are needed due to increasing number of multicomponent formulations, biotherapeutic products and samples of complex matrix in que. Number of Ultraviolet (UV) spectrophotometric methods used for these purpose. Different types of UV spectrometric methods developed on the basis of principle of additivity, absorbance difference, processing absorption spectra. The aim of this review is to present information on simultaneous equation method, difference spectrophotometry, derivative spectrophotometry, absorbance ratio spectra, derivative ratio spectra, successive ratio - derivative spectra, Q-absorbance ratio method, absorptivity factor method, dual wavelength method, absorption factor method, multivariate chemometric methods, and isosbestic point method. A brief summary on theories, mathematical background and some applications of these methods are presented here.

scholarly journals Validation of an HPLC method for the simultaneous determination of eletriptan and UK 120.413

2006 ◽  
Vol 71 (11) ◽  
pp. 1195-1205 ◽  
Author(s):  
Mira Zecevic ◽  
Biljana Jocic ◽  
Snezana Agatonovic-Kustrin ◽  
Ljiljana Zivanovic
Keyword(s):  
Mobile Phase ◽  
Analytical Procedure ◽  
Internal Standard ◽  
Correlation Coefficients ◽  
Hplc Method ◽  
Control Analysis ◽  
Internal Standard Method ◽  
Rp Hplc ◽  
Good Repeatability

Arapid and sensitive RPHPLCmethod was developed for the routine control analysis of eletriptan hydrobromide and its organic impurity UK 120.413 in Relpax? tablets. The chromatography was performed at 20?C using a C18 XTerra ? (5 ?m, 150 x 4,6 mm) column at a flow rate 1.0 ml/min. The drug and its impurity were detected at 225 nm. The mobile phase consisted of TEA (1 %) - methanol (67.2:32.8 v/v), the pH of which was adjusted to 6.8 with 85 % orthophosphoric acid. Quantification was accomplished by the internal standard method. The developed RP HPLC method was validated by testing: accuracy, precision, repeatability, specificity, detection limit, quantification limit, linearity, robustness and sensitivity. High linearity of the analytical procedure was confirmed over the concentration range of 0.05 - 1.00 mg/ml for eletriptan hydrobromide and from 0.10 - 1.50 ?g/ml for UK 120.413, with correlation coefficients greater than r = 0.995. The low value of the RSD expressed the good repeatability and precision of the method. Experimental design and a response surface method were used to test robustness of the analytical procedure and to evaluate the effect of variation of the method parameters, namely the mobile phase composition, pH and temperature. They showed small deviations from the method setting. The good recovery and low RSD confirm the suitability of the proposed RP HPLC method for the routine determination of eletriptan hydrobromide and its impurity UK 120.413 in Relpax? tables.

scholarly journals Determination of Carbamazepine and Its Impurities Iminostilbene and Iminodibenzyl in Solid Dosage Form by Column High-Performance Liquid Chromatography

2010 ◽  
Vol 93 (4) ◽  
pp. 1059-1068 ◽  
Author(s):  
Predrag Lj Džodić ◽  
Ljiljana J ivanovi ◽  
Ana D Proti ◽  
Mira L Zeevi ◽  
Biljana M Joci
Keyword(s):  
Mobile Phase ◽  
High Performance ◽  
Dosage Form ◽  
Internal Standard ◽  
Hplc Method ◽  
Solid Dosage ◽  
Rp Hplc ◽  
Good Repeatability ◽  
Chemometric Approach

Abstract An accurate and precise RP-HPLC method was developed and validated for the determination of carbamazepine and its impurities iminostilbene and iminodibenzyl in a tablet formulation with fluphenazine as an internal standard. Buffermethanol (50 + 50, v/v) was used as the mobile phase. During validation, specificity, linearity, precision, accuracy, LOD, LOQ, and robustness of the method were tested. The method was proven to be specific against placebo interference. Linearity was evaluated over the concentration range of 100500, 0.050.25, and 0.10.5 g/mL, and the r values were 0.9994, 0.9997, and 0.9979 for carbamazepine, iminostilbene, and iminodibenzyl, respectively. Intraday precision of the method was good, and RSD was below 2 for all analytes. The accuracy of the method ranged from 100.69 to 102.10, 99.76 to 102.66, and 99.26 to 100.08 for carbamazepine, iminostilbene, and iminodibenzyl, respectively. LOD was 0.0125, 0.025, and 0.05 g/mL and LOQ was 0.05, 0.05, and 0.1 g/mL for carbamazepine, iminostilbene, and iminodibenzyl, respectively. Robustness of the method was proven by using a chemometric approach. The method was successfully applied to the analysis of commercially available carbamazepine tablets and showed good repeatability, with RSD below 2.

APPLICATION OF HPTLC AND RP-HPLC METHODS FOR SIMULTANEOUS ESTIMATION OF OFLOXACIN AND PREDNISOLONE ACETATE IN OPHTHALMIC DOSAGE FORM

INDIAN DRUGS ◽  
2015 ◽  
Vol 52 (05) ◽  
pp. 17-26
Author(s):  
M. L Chavhan ◽  
◽  
A. S Patil ◽  
S. J Surana ◽  
A. A. Shirkhedkar
Keyword(s):  
Mobile Phase ◽  
Dosage Form ◽  
Internal Standard ◽  
Prednisolone Acetate ◽  
Simultaneous Estimation ◽  
Hplc Separation ◽  
Potassium Dihydrogen ◽  
Rp Hplc ◽  
Ophthalmic Formulation

Two simple, rapid, precise, accurate and robust (HPTLC and RP-HPLC) methods have been established for simultaneous determination of ofloxacin and prednisolone acetate in its combined ophthalmic formulation. HPTLC separation of two drugs was accomplished on a HPTLC aluminum-backed layer of silica gel 60 F254 using n-butanol: methanol: ammonia (60:10:30% V/V/V) as a mobile phase. The densitometric scanning was performed at 275 nm which showed Rf 0.43 for ofloxacin and 0.78 for prednisolone acetate, respectively. RP-HPLC separation of the two drugs was achieved on LC-GC Qualisil BDS C-18 column using mobile phase methanol: acetonitrile: 0.02 M potassium dihydrogen ortho-phosphate anhydrous (50:15:35% V/V/V), pH adjusted to 4.5 with triethylamine. Detection of both drugs was done at 275 nm. Aspirin was used as an internal standard (IS). The retention time for ofloxacin, prednisolone acetate and aspirin (IS), was found to be 4.36 min. and 6.60 min and 3.55 min, respectively. The proposed methods were successfully applied for the determination of both drugs in bulk and in combined ophthalmic formulation. Assay of both these methods were compared using student t-test.

scholarly journals VALIDATED GRADIENT STABILITY INDICATING RP-HPLC METHOD FOR THE SIMULTANEOUS QUANTIFICATION OF 11 RELATED SUBSTANCES IN THE COMBINED DOSAGE FORMS OF LAMIVUDINE AND TENOFOVIR DISOPEOXIL FUMARATE

2017 ◽  
Vol 9 (4) ◽  
pp. 61 ◽  
Author(s):  
C. Babu ◽  
N. Devanna ◽  
K. V.n. Suresh Reddy
Keyword(s):  
Mobile Phase ◽  
Ammonium Acetate ◽  
Dosage Forms ◽  
Hplc Method ◽  
Forced Degradation ◽  
Stability Indicating ◽  
Simultaneous Quantification ◽  
Related Substances ◽  
Drug Substances ◽  
Rp Hplc

Objective: Development of a stability-indicating reverse phase liquid chromatographic (RP-HPLC) method for the simultaneous quantification of 11 impurities in the combined dosage forms of lamivudine and tenofovir disoproxil fumarate drug substances.Methods: Efficient chromatographic separation of all analytes was achieved on a Waters X-terra RP18 column (150 x 4.6 mm, 3.5 mm) using mobile phase A (ammonium acetate buffer, pH adjusted to 5.0±0.05 with dilute orthophosphoric acid) and mobile phase B (mixture of methanol and ammonium acetate buffer in the ratio of 20:80) with the flow rate of 1.0 ml/min in gradient elution mode at 260 nm.Results: The method was validated in terms of the limit of detection, limit of quantification, linearity, accuracy, precision and robustness according to the international conference on harmonisation (ICH Q2R1). Regression analysis showed that the correlation coefficient (r2) is greater than 0.997 for individual active drug substances as well as their related substances. The method has proven very accurate (94.6 % to 108.2 % with % RSD not more than 4.9), highly precise (% RSD of the Intra-day and the inter-day study was not more than 8.9) and robust enough to deliver accurate results, when the chromatographic conditions were altered intentionally. Forced degradation studies were conducted in acidic, basic, thermal, photolytic, humid and peroxide stress conditions, where all the degradation peaks were monitored. Highest degradation of lamivudine was observed under oxidative stress condition and tenofovir was more susceptible to degradation under acidic and alkaline conditions.Conclusion: The present method is able to separate all the related compounds with each other and with the main drug substances with the resolution more than 2.0. The test solution was found to be stable in diluent up to 24 h. The mass balance of forced degradation of formulations, close to 99 %, made this method as a stability indicating method.

scholarly journals Application of RP-HPLC method for the simultaneous determination of cetirizine in the presence of quinolones

2021 ◽  
Vol 7 (1) ◽  
Author(s):  
Hina Shamshad ◽  
Agha Zeeshan Mirza
Keyword(s):  
Human Serum ◽  
Simultaneous Determination ◽  
Flow Rate ◽  
Mobile Phase ◽  
Diclofenac Sodium ◽  
Internal Standard ◽  
Hplc Method ◽  
Rp Hplc ◽  
Ich Guidelines

Abstract Background Present work describes a fast, simple, and sensitive procedure for the simultaneous determination of cetirizine in the presence of quinolones using diclofenac sodium as an internal standard. The present work was designed to analyze these compounds in pharmaceutical and clinical labs being economical for use. Results The mobile phase consisted of the simple composition of methanol, acetonitrile, and water in a ratio of 50:20:30 with a pH adjusted to 3.1 at a flow rate of 1 mL min−1. The UV detection was performed at 225 nm. The linearity was assessed over the range of 2.5–50 μg mL−1 for all drugs. The parameters such as accuracy, precision, linearity (>0.999), and sensitivity were satisfactory. Conclusion The method was equally applicable for formulation and human serum with recovery values between 95 and 105%. The results of the method were validated statistically according to ICH guidelines.

scholarly journals Development and Validation of Spectrophotometric Methods for Simultaneous Estimation of Valsartan and Hydrochlorothiazide in Tablet Dosage Form

2014 ◽  
Vol 2014 ◽  
pp. 1-6 ◽  
Author(s):  
Monika L. Jadhav ◽  
Manoj V. Girase ◽  
Shripad K. Tidme ◽  
Manish S. Junagade
Keyword(s):  
Dosage Form ◽  
Pharmaceutical Formulations ◽  
Simultaneous Equation ◽  
Ratio Method ◽  
Simultaneous Estimation ◽  
Spectrophotometric Methods ◽  
Absorbance Ratio ◽  
Standard Additions ◽  
Development And Validation ◽  
Tablet Dosage

Two UV-spectrophotometric methods have been developed and validated for simultaneous estimation of valsartan and hydrochlorothiazide in a tablet dosage form. The first method employed solving of simultaneous equations based on the measurement of absorbance at two wavelengths, 249.4 nm and 272.6 nm, λmax for valsartan and hydrochlorothiazide, respectively. The second method was absorbance ratio method, which involves formation of Q-absorbance equation at 258.4 nm (isoabsorptive point) and also at 272.6 nm (λmax of hydrochlorothiazide). The methods were found to be linear between the range of 5–30 µg/mL for valsartan and 4–24 μg/mL for hydrochlorothiazide using 0.1 N NaOH as solvent. The mean percentage recovery was found to be 100.20% and 100.19% for the simultaneous equation method and 98.56% and 97.96% for the absorbance ratio method, for valsartan and hydrochlorothiazide, respectively, at three different levels of standard additions. The precision (intraday, interday) of methods was found within limits (RSD<2%). It could be concluded from the results obtained in the present investigation that the two methods for simultaneous estimation of valsartan and hydrochlorothiazide in tablet dosage form are simple, rapid, accurate, precise and economical and can be used, successfully, in the quality control of pharmaceutical formulations and other routine laboratory analysis.

scholarly journals Optimization and Validation of an RP-HPLC Method for Analysis of Hydrocortisone Acetate and Lidocaine in Suppositories

2010 ◽  
Vol 93 (1) ◽  
pp. 102-107 ◽  
Author(s):  
Biljana Jancic-Stojanović ◽  
Andjelija Malenović ◽  
Slavko Marković ◽  
Darko Ivanović ◽  
Mirjana Medenica
Keyword(s):  
Particle Size ◽  
Response Surface Methodology ◽  
Mobile Phase ◽  
Orthophosphoric Acid ◽  
Internal Standard ◽  
Hplc Method ◽  
Hydrocortisone Acetate ◽  
Rp Hplc ◽  
Method Optimization

Abstract An RP-HPLC method has been optimized and validated for the simultaneous determination of hydrocortisone acetate and of lidocaine in suppositories. For the method optimization, response surface methodology was applied, and the obtained model was tested using analysis of variance. The optimal separations were conducted on a Beckman-Coulter 150 4.6 mm, 5 µm particle-size column at 20C. The mobile phase was methanolwater (65 + 35, v/v), pH adjusted to 2.5 with 85% orthophosphoric acid, with a flow rate of 1.0 mL/min. UV detection was performed at 250 nm. Phenobarbital was used as an internal standard. The method was validated for selectivity, linearity, precision, and robustness.

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