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.

scholarly journals Stability Indicating RP-HPLC Method for Determination of Valsartan in Pure and Pharmaceutical Formulation

2010 ◽  
Vol 7 (1) ◽  
pp. 246-252 ◽  
Author(s):  
S. K. Patro ◽  
S. K. Kanungo ◽  
V. J. Patro ◽  
N. S. K. Choudhury
Keyword(s):  
Linear Response ◽  
Mobile Phase ◽  
Hplc Method ◽  
Forced Degradation ◽  
Control Analysis ◽  
Solution Stability ◽  
Stability Indicating ◽  
Quality Control Analysis ◽  
Rp Hplc

A simple, rapid and accurate and stability indicating RP-HPLC method was developed for the determination of valsartan in pure and tablet forms. The method showed a linear response for concentrations in the range of 50-175 µg/mL using 0.01 M NH4H2PO4(pH 3.5) buffer: methanol [50:50] as the mobile phase with detection at 210 nm and a flow rate of 1 mL/min and retention time 11.041 min. The method was statistically validated for accuracy, precision, linearity, ruggedness, robustness, forced degradation, solution stability and selectivity. Quantitative and recovery studies of the dosage form were also carried out and analyzed; the % RSD from recovery studies was found to be less than 1. Due to simplicity, rapidity and accuracy of the method, we believe that the method will be useful for routine quality control analysis.

Simultaneous determination of Sulphadoxine and Pyrimethamine by taking Tolterodine as an internal standard in Pharmaceutical dosage form by RP-HPLC

2021 ◽  
pp. 145-150
Author(s):  
Sushil D. Patil ◽  
Pravin B. Shelke ◽  
Priti Aher ◽  
Maswood Ahmed Hafizur Rahman
Keyword(s):  
Simultaneous Determination ◽  
Dosage Form ◽  
Internal Standard ◽  
Hplc Method ◽  
Control Analysis ◽  
Pharmaceutical Dosage Form ◽  
Quality Control Analysis ◽  
Rp Hplc ◽  
Sulphadoxine Pyrimethamine

A simple, rapid, economic, sensitive and precise HPLC method has been developed for the simultaneous determination of Sulphadoxine and Pyrimethamine in pharmaceutical dosage form by taking Tolterodine as an internal standard. The method was carried out using Phenomenex C18 (4.6ID × 250mm; 5µm) column and mobile phase comprised of methanol and Phosphate Buffer in proportion of ratio 60:40 v/v. The flow rate was 1.0mL/min and detection was carried out at 276nm. The retention time of Sulphadoxine, Pyrimethamine and Tolterodine were found to be 2.967, 4.058 and 6.908 respectively. Linearity of Sulphadoxine and Pyrimethamine in the range of 2 to 12μg/mL and 4 to 24μg/mL respectively. The % recoveries of Sulphadoxine and Pyrimethamine were found to be in between 99.93% to 99. 96 % respectively. The proposed method is suitable for the routine quality control analysis for simultaneous determination of Sulphadoxine and Pyrimethamine was in bulk and pharmaceutical dosage form.

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 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.

scholarly journals Simple RP-HPLC method for determination of triple drug combination of valsartan, amlodipine and hydrochlorothiazide in human plasma

2012 ◽  
Vol 62 (1) ◽  
pp. 45-58 ◽  
Author(s):  
Ritesh Sharma ◽  
Shyam Pancholi
Keyword(s):  
Human Plasma ◽  
Drug Combination ◽  
Mobile Phase ◽  
Internal Standard ◽  
Hplc Method ◽  
Ammonium Formate ◽  
Good Reproducibility ◽  
Phase Gradient ◽  
Rp Hplc

Simple RP-HPLC method for determination of triple drug combination of valsartan, amlodipine and hydrochlorothiazide in human plasma A simple RP-HPLC method for the quantification of valsartan (VAL), amlodipine (AML) and hydrochlorothiazide (HCT) in human plasma was developed and validated. VAL, AML and HCT were resolved using a Gemini C18 column and mobile phase gradient starting from 20 % acetonitrile and 80 % 10 mmol L-1 ammonium formate (V/V, pH 3.5 ± 0.2, by formic acid) to 70 % acetonitrile and 30 % 10 mmol L-1 ammonium formate, over 20 minutes, with a flow rate of 1 mL min-1. The samples were purified by protein precipitation and extraction. Telmisartan was used as internal standard. The method was validated according to USFDA and EMEA guidelines with good reproducibility and linear responses R = 0.9985 (VAL), 0.9964 (AML), and 0.9971 (HCT). RSDs of intra- and inter-day precision ranged 2.2-8.1 and 4.6-11.7 %, respectively, for all three drugs. Mean extraction recoveries of three QCs for the triple drug combination were 76.5 (VAL), 72.0 (AML) and 73.0 (HCT) % for human plasma. Although the LC-MS/MS method is more sensitive than HPLC, HPLC is still suitable for preliminary pharmacokinetic study. The experiments performed demostrated that simultaneous determination of all components of the triple drug combination in human plasma can be done by this method. Proposed method can be also used for guidance to the LC-MS/MS method.

scholarly journals Simultaneous Determination of Lamivudine, Zidovudine and Abacavir in Tablet Dosage Forms by RP HPLC Method

2010 ◽  
Vol 7 (1) ◽  
pp. 180-184 ◽  
Author(s):  
D. Anantha Kumar ◽  
G. Srinivasa Rao ◽  
J. V. L. N. Seshagiri Rao
Keyword(s):  
Simultaneous Determination ◽  
Internal Standard ◽  
Dosage Forms ◽  
Hplc Method ◽  
Control Analysis ◽  
Potassium Dihydrogen ◽  
Quality Control Analysis ◽  
Rp Hplc ◽  
Tablet Dosage

A simple, accurate and reproducible RP-HPLC method has been developed for the simultaneous determination of lamivudine, zidovudine and abacavir in tablet dosage forms. Chromatography was carried out on a HiQ Sil C 18 V column using a mobile phase consisting of 0.01 M potassium dihydrogenortho-phosphate (pH 3.0) and methanol (55:45 v/v) at a flow rate of 0.8 mL/min. The detection was made at 272 nm and stavudine was used as the internal standard for this study. The retention times for lamivudine, abacavir and zidovudine were found to be 3.8, 6.3, 8.1 min. respectively. The calibration curves were linear over the range 5-250 μg/mL for both zidovudine and abacavir and 5-140 μg/mL for lamivudine. The proposed method was validated as per ICH and USP guidelines and it was found suitable for the routine quality control analysis of the drugs in tablet dosage forms.

scholarly journals Comparative validation of HPLC, densitometric and videodensitometric determination of lamotrigine in pharmaceutical

2014 ◽  
Vol 27 (4) ◽  
pp. 258-262
Author(s):  
Beata Paw
Keyword(s):  
Quality Control ◽  
Flow Rate ◽  
Mobile Phase ◽  
Internal Standard ◽  
Correlation Coefficients ◽  
Hplc Method ◽  
Densitometric Detection ◽  
Precision And Accuracy ◽  
Comparative Validation

Abstract Simple, sensitive, precise and accurate HPLC, densitometric and videodensitometric methods for determination of lamotrigine in tablet forms were developed and validated. The HPLC method was carried out using a Symmetry C8 column and a mobile phase acetonitrile-phosphate buffer pH 2.80 (25:75, v/v), with a flow rate of 1 mL/min, and UV detection at 210 nm. Ethosuximide was used as the internal standard. Densitometric and videodensitometric analysis was performed on silica gel 60 F254 plates, in horizontal chambers, with methanol-chloroform-ammonia (25%) 1.5:7.5:1, (v/v) as mobile phase. Densitometric detection was performed at 225 nm and at 315 nm, and videodeoscanning at 254 nm. Calibration plots were constructed in the range 0.5-10 μg/spot, with good correlation coefficients r > 0.99 for both methods. The precision and accuracy of all elaborated methods were compared. Finally, the developed methods were applied for the quality control of lamotrigine tablets.

scholarly journals RAPID AND ECONOMICAL QUANTITATIVE DETERMINATION OF SEVERAL ANTIHYPERTENSIVE AGENTS IN PRESENCE OF HYDROCHLOROTHIAZIDE BY ISOCRATIC REVERSED-PHASE HIGH-PERFORMANCE LIQUID CHROMATOGRAPHY IN THEIR PHARMACEUTICAL PREPARATIONS

2017 ◽  
Vol 10 (12) ◽  
pp. 155
Author(s):  
Panchumarthy Ravisankar ◽  
Devala Rao G ◽  
Md Shaheem Sulthana ◽  
Supriya K ◽  
Mounika G ◽  
...  
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
Quantitative Determination ◽  
Mobile Phase ◽  
High Performance ◽  
Hplc Method ◽  
Control Analysis ◽  
Rp Hplc ◽  
Relative Standard

Objective: Objective of the present investigation is to develop a speedy isocratic reverse phase high-performance liquid chromatography (RP-HPLC) method for the separation and quantitative determination of 5 angiotensin II - receptor antagonists, namely, telmisartan, losartan, valsartan, olmesartan, irbesartan, and atenolol along with thiazide diuretics mostly hydrochlorothiazide (HCTZ).Methods: RP-HPLC method was evolved using Welchrom C18 column (4.6 × 250 mm, 5 μm) as a stationary phase with the mobile phase comprising a variety of phosphate buffer with pH-3.3 and acetonitrile in the proportion of 50:50 v/v. The mobile phase was pumped at a current rate of 1 mL/minute. The detection wavelength was carried out at 230 nm.Results: The total run time was 6 minutes and the elution window of only 3 minutes. The peaks were eluted with decorous resolution. The calibration curves were linear (r2=0.9998) in all cases. The percentage relative standard deviation (RSD%) was <2% and average recovery was above 99.95%. The method was validated specificity, precision, and accuracy. High recovery values and low RSD% prove that this method is very accurate and reproducible. The developed method was applied to the estimation of the above-said drugs in binary combinations from different manufacturers which were a good agreement with label claim.Conclusion: The important advantage of developed method was that the five individual drugs can be determined on a single chromatographic system without alteration in detection wavelength and mobile phase composition. This novel method was statistically validated as per ICH guidelines. The optimized method proved to be linear, accurate, and robust. Hence, the above said proposed method was found to be a rapid tool for the routine determination of the above-said drugs in alone or combination with HCTZ in quality control analysis without interference of excipients.

RP-HPLC METHOD FOR SIMULTANEOUS ESTIMATION OF ASPIRIN AND OMEPRAZOLE IN BINARY COMBINATION

INDIAN DRUGS ◽  
2018 ◽  
Vol 55 (08) ◽  
pp. 38-43
Author(s):  
A. M Kashid ◽  
◽  
S. V. Tathe ◽  
S. G. Sahoo ◽  
A. B. Ghatge ◽  
...  
Keyword(s):  
Mobile Phase ◽  
Correlation Coefficients ◽  
Hplc Method ◽  
Simultaneous Estimation ◽  
Sodium Acetate Buffer ◽  
Rp Hplc ◽  
Ich Guidelines ◽  
Precision Study ◽  
The Mean

A simple, accurate, rapid and precise RP-HPLC method for the simultaneous estimation of aspirin and Omeprazole in binary mixture has been developed and validated. The drugs were resolved using HPLC column (ACE 250 x 4.6 mm C18 column) with mobile phase of HPLC grade methanol: Sodium acetate buffer (70:30 v/v) at a flow rate of 1 mL/min. The retention times of aspirin and omeprazole were 3.10 ± 0.3min and 5.01 ± 0.02min with UV detection at 230 nm. The method was validated with respect to linearity, sensitivity, accuracy, precision and robustness as per the International Conference on Harmonization (ICH) guidelines. The method was specific and it was observed that no interference with diluents. The linearity was established over the concentration range of 40-140μg/ml and 20-120μg/mL with correlation coefficients (r2) 0.9998 and 0.9986 for aspirin andomeprazole magnesium respectively. The mean recoveries were found to be in the range of 97.05%-99.75% and 97.21% -98.76% for aspirin and omeprazole respectively. The % R.S.D. values for intra-day precision study and inter-day study were <1.0%, confirming that the method is precise. The method can be successfully employed for the simultaneous determination of aspirin and omeprazole.

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