RP-HPLC determination of dissociation constant using solely aqueous mobile phase

2017 ◽  
Vol 134 ◽  
pp. 143-148 ◽  
Author(s):  
Tereza Volná ◽  
Kamil Motyka ◽  
Jan Hlaváč
2019 ◽  
Vol 9 (o3) ◽  
Author(s):  
Imad Tarek Hanoon ◽  
Abed Mohammed Daheir AL-Joubory 2 ◽  
Marwa Mohamed Saied 3

A simple , specific, accurate and precise RP-HPLC method was developed for determination of Irbesartan (IRB) in pharmaceutical dosage forms in tablets products and sachet using symmetry (L 1 ) column at 30°C . The signal was detected at 225 nm. A mobile phase dissolve 0.5 g of buffer potassium phosphate in 100 ml distilled water and adjust pH 2.7 , methanol and acetonitrile at ratio (40 :30 :30 ) . and flow rate 1.2ml/min -1 at pH=7.2 a mobile phase The percent recovery was detected 101 % and the linearity of concentration was 10-50 µg.ml -1 and supported this method by using (FT.I.R.) spectrum method for organic spectrophotometer to prove the chemical structure of this drug and some physical properties . we are obtained the result is identical of other literature . The proposed method was applied successfully for determination of the IRB in tablets products.


Separations ◽  
2021 ◽  
Vol 8 (1) ◽  
pp. 5
Author(s):  
Mohd Afzal ◽  
Mohd. Muddassir ◽  
Abdullah Alarifi ◽  
Mohammed Tahir Ansari

A highly specific, accurate, and simple RP-HPLC technique was developed for the real-time quantification of domperidone (DOMP) and lansoprazole (LANS) in commercial formulations. Chromatographic studies were performed using a Luna C8(2), 5 μm, 100Å, column (250 × 4.6 mm, Phenomenex) with a mobile phase composed of acetonitrile/2 mM ammonium acetate (51:49 v/v), pH 6.7. The flow rate was 1 mL·min−1 with UV detection at 289 nm. Linearity was observed within the range of 4–36 µg·mL−1 for domperidone and 2–18 µg·mL−1 for lansoprazole. Method optimization was achieved using Box-Behnken design software, in which three key variables were examined, namely, the flow rate (A), the composition of the mobile phase (B), and the pH (C). The retention time (Y1 and Y3) and the peak area (Y2 and Y4) were taken as the response parameters. We observed that slight alterations in the mobile phase and the flow rate influenced the outcome, whereas the pH exerted no effect. Method validation featured various ICH parameters including linearity, limit of detection (LOD), accuracy, precision, ruggedness, robustness, stability, and system suitability. This method is potentially useful for the analysis of commercial formulations and laboratory preparations.


2006 ◽  
Vol 3 (1) ◽  
pp. 60-64 ◽  
Author(s):  
P. Venkata Reddy ◽  
B. Sudha Rani ◽  
G. Srinu Babu ◽  
J. V. L. N. Seshagiri Rao

A reverse phase HPLC method is developed for the determination of Raloxifene in pharmaceutical dosage forms. Chromatography was carried out on an inertsil C18 column using a mixture of acetonitrile and phosphate buffer (30:70 v/v) as the mobile phase at a flow rate of 1 mL/min. Detection was carried out at 290 nm .The retention time of the drug was 10.609 min. The method produced linear responses in the concentration range of 0.5-200 µg/mL of Raloxifene. The method was found to be applicable for determination of the drug in tablets.


INDIAN DRUGS ◽  
2014 ◽  
Vol 51 (12) ◽  
pp. 32-36
Author(s):  
T. Vishalakhi ◽  
◽  
S. K Kumar ◽  
K Sujana ◽  
P Rani

A simple validated RP HPLC method for the estimation of rizatriptan benzoate in pharmaceutical dosage form and bulk was developed for routine analysis. This method was developed by selecting Agilent TC C18 (250 x 4.6 mm, 5 μ) column as stationary phase and acrylonibrile:water (45:55), pH adjusted to 3, as mobile phase. Flow rate of mobile phase was maintained at 4: 1 mL/min at ambient temperature throughout the experiment. Quantification was achieved with ultraviolet (DAD) detection at 220 nm. The retention time obtained for rizatriptan was 2.8 min. The detector response was linear in the concentration range of 2-25μg/mL. This method was validated and shown to be specific, sensitive, precise, linear, accurate, rugged and robust. Hence, this method can be applied for routine quality control of rizatriptan benzoate in dosage forms as well as in bulk drug.


2021 ◽  
Vol 66 (3) ◽  
pp. 172-176
Author(s):  
Lyubov Borisovna Kalikova ◽  
E. R. Boyko

Adenine nucleotides (ATP, ADP and AMP) play a central role in the regulation of metabolism and energy: they provide the energy balance of the cell, determine its redox state, act as allosteric effectors of a number of enzymes, modulate signaling and transcription factors and activate oxidation or biosynthesis substrates. A large number of methods have been developed to determine the level of ATP, ADP and AMP, but the most universal and effective method for the separation and analysis of complex mixtures is the reversed-phase high-performance liquid chromatography method (RP-HPLC). The aim of this study is to determine the optimal conditions for the qualitative separation and quantitative determination of standard solutions of ATP (1 mmol/l), ADP (0,5 mmol/l) and AMP (0,1 mmol/l) by RP-HPLC. The degree of separation of adenine nucleotides was estimated by the time of peak output in the chromatogram. To achieve the goal, the following tasks were set: assess the effect of the temperature of the analysis on the separation and change of the release time of the analytes in the chromatogram; determine the most optimal composition of the mobile phase for the separation of ATP, ADP and AMP in the chromatogram (the content of the organic solvent in the solution); to identify the effect of pH of the mobile phase on the separation of standard solutions of adenine nucleotides; set the optimal molarity of the mobile phase for the separation of ATP, ADP and AMP in the chromatogram. It was found that the temperature of the analysis does not affect the quality of peak separation, while the composition and pH of the mobile phase have a significant effect on the complete and clear separation of the studied nucleotides in the chromatogram. It was determined that the analysis temperature of 37°C and the mobile phase of 0.05 M KH2PO4 (pH 6.0) are optimal for separating the peaks of adenine nucleotides.


Author(s):  
Muhammad Fawad Rasool ◽  
Umbreen Fatima Qureshi ◽  
Nazar Muhammad Ranjha ◽  
Imran Imran ◽  
Mouqadus Un Nisa ◽  
...  

AbstractTh accurate rapid, simple and selective reversed phase high performance liquid chromatography (RP-HPLC) has been established and validated for the determination of captopril (CAP). Chromatographic separation was accomplished using prepacked ODSI C18 column (250 mm × 4.6 mm with 5 μm particle size) in isocratic mode, with mobile phase consisting of water: acetonitrile (60:40 v/v), pH adjusted to 2.5 by using 85% orthophosphoric acid at a flow rate of 1 mL/min and UV detection was performed at 203 nm. RP-HPLC method used for the analysis of CAP in mobile phase and rabbit plasma was established and validated as per ICH-guidelines. It was carried out on a well-defined chromatographic peak of CAP was established with a retention time of 4.9 min and tailing factor of 1.871. The liquid–liquid extraction method was used for extraction of CAP from the plasma. Excellent linearity (R2 = 0.999) was shown over range 3.125–100 µg/mL with mean percentage recoveries ranges from 97 to 100.6%. Parameters of precision and accuracy of the developed method meet the established criteria. Intra and inter-day precision (% relative standard deviation) study was also performed which was less than 2% which indicate good reproducibility of the method. The limit of detection (LOD) and quantification for the CAP in plasma were 3.10 and 9.13 ng/mL respectively. The method was suitably validated and successfully applied to the determination of CAP in rabbit plasma samples.


Author(s):  
K. S Ashutosh ◽  
D. Manidipa ◽  
R. J. V. L. N. Seshagiri ◽  
S. D. Gowri

The RP-HPLC separation was carried out by reverse phase chromatography on a Symmetry C18 (4.6 x 150 mm, 3.5 μm, make: XTerra) with a mobile phase composed of sodium dihydrogen ortho phosphate [pH 2.5] and acetonitrile in the ratio of 30:70 v/v in an isocratic mode at a flow rate of 1.2 mL/min. The run time was maintained for 8.0 min. The detection was monitored at 236 nm. The accuracy was calculated in human plasma and the % recovery was found 99.80 - 99.85 for famotidine and 99.56 -99.85.5 for ibuprofen and reproducibility was found to be satisfactory. The calibration curve for famotidine in human plasma was linear over 3.32 to 6.65 μg/mL and 100- 200 μg/mL for ibuprofen in human plasma respectively. The inter-day and intra-day precision in human plasma was found within limits. The proposed method has adequate sensitivity, reproducibility, and specificity for the determination of famotidine and ibuprofen in plasma. The LLOQ obtained by the proposed method in human plasma were 1.24 and 5.0 μg/mL for famotidine and ibuprofen respectively. The proposed method is simple, fast, accurate, and precise for the quantification of famotidine and ibuprofen in plasma as per the ICH guidelines.Kathmandu University Journal of Science, Engineering and TechnologyVol. 12, No. I, June, 2016, Page: 34-48


2010 ◽  
Vol 7 (1) ◽  
pp. 246-252 ◽  
Author(s):  
S. K. Patro ◽  
S. K. Kanungo ◽  
V. J. Patro ◽  
N. S. K. Choudhury

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.


INDIAN DRUGS ◽  
2018 ◽  
Vol 55 (03) ◽  
pp. 32-42
Author(s):  
G. P Wani ◽  
◽  
S. B Jadhav

Simple, rapid, precise, accurate RP-HPLC and HPTLC methods have been developed and validated for ivermectin in bulk and its marketed formulation. RP-HPLC method for drug was achieved on Grace C18 (250 mm X 4.6 ID, Particle size; 5 μ) column using mobile phase acetonitrile: 10 mM phosphate buffer (95:05 v/v) pH adjusted to 3 with o-phosphoric acid. Detection of drug was done at 245 nm. The retention time was found to be 5.83 min. HPTLC method for ivermectin was accomplished on a precoated silica gel aluminium plate 60F-254 (CAMAG Linomat 5), using toluene: methanol: glacial acetic acid (8:2:0.1 v/v/v) as a mobile phase. The densitometric scanning was performed at 245 nm which showed Rf 0.46 for ivermectin. The stress testing of the drug individually was carried out under acidic, alkaline, oxidation, photo-stability and thermal degradation conditions. The proposed methods were successfully applied for the determination of drug in bulk and its marketed formulation.


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