DEVELOPMENT AND VALIDATION OF LIQUID CHROMATOGRAPHIC METHOD FOR SIMULTANEOUS ESTIMATION OF STRYCHNINE AND GALLIC ACID

INDIAN DRUGS ◽  
2018 ◽  
Vol 55 (06) ◽  
pp. 46-50
Author(s):  
V. V. Khanvilkar ◽  
◽  
M Toraskar
Keyword(s):  
Gallic Acid ◽  
Potassium Dihydrogen Phosphate ◽  
Hplc Method ◽  
Simultaneous Estimation ◽  
Dihydrogen Phosphate ◽  
Potassium Dihydrogen ◽  
Rp Hplc ◽  
Liquid Chromatographic Method ◽  
Development And Validation ◽  
Liquid Chromatographic

An accurate, precise and robust RP-HPLC method was developed for the simultaneous estimation of strychnine and gallic acid. The markers were resolved using HiQ C18HS column with methanol and potassium dihydrogen phosphate buffer (10 mM, pH 3) (60:40 V/V) as mobile phase at flow rate of 1 mL per minute and run time of 6 minutes. Retention times of strychnine and gallic acid were 3 and 4.7 minutes, respectively at 264 nm. The linearity range for strychnine and gallic acid was found to be 0.5-3 μg/mL and 1-3.5 µg/mL, respectively with coefficient of linear regression greater than 0.99 for both the markers. The developed method was validated as per ICH Q2 (R1) guidelines and the results obtained were satisfactory. The method was applied for quantification of markers in marketed and In-house formulations of Agnitundi Vati, a polyherbal ayurvedic formulation. The developed method thus could be used for standardization of Agnitundi Vati and other herbal preparations containing these two markers.

scholarly journals Development and Validation of RP-HPLC Method for Estimation of Teneligliptin and its Impurity in Tablet

2021 ◽  
Vol 69 (02) ◽  
Author(s):  
Bhoomi Dineshkumar Patel ◽  
Nidhi J. Dharsandiya ◽  
Ankit Chaudhary
Keyword(s):  
Present Method ◽  
Mobile Phase ◽  
Potassium Dihydrogen Phosphate ◽  
Hplc Method ◽  
Simultaneous Estimation ◽  
Dihydrogen Phosphate ◽  
Potassium Dihydrogen ◽  
Rp Hplc ◽  
Development And Validation ◽  
Tablet Dosage

The objective of the study is a simple, precise and accurate stability RP-HPLC method has been developed and subsequently validated for the estimation of Teneligliptin and its impurity in tablet formulation. The adequate separation was carried out using Grace Smart C18 column (250mm x 4.6mm, 5?m particle size), mixture of 0.05M Potassium dihydrogen phosphate PH 4.0 and Acetonitrile 80:20 % v/v as a mobile phase with a flow rate of 1 ml/min and the effluent was monitored at 242 nm using PDA detector. The retention time of Teneligliptin, Impurity B and Impurity G were 7.443 min, 6.650 min and 8.473 min respectively. Linearity for Teneligliptin, Impurity B and Impurity G were found in the range of 500-3000 µg/ml (R2 = 0.998), 5-15 µg/ml (R2 = 0.994) and 5-15 µg/ml (R2 = 0.998) respectively. The accuracy of the present method was evaluated at 50%, 100% and 150%. The % recoveries of drug were found to be in range of 99.315 ± 0.283 for Teneligliptin. Precision studies were carried out and the RSD values were less than two. The method was found to be robust. The proposed method was found to be specific, accurate, precise and robust can be used for simultaneous estimation of these drugs in tablet dosage form.

scholarly journals Validated stability-indicating RP-HPLC method for simultaneous estimation of cilnidipine and chlorthalidone in tablet dosage form

2020 ◽  
Vol 11 (SPL4) ◽  
pp. 2435-2441
Author(s):  
Ashok B. Patel ◽  
Amitkumar J. Vyas ◽  
Shital Faldu ◽  
Arvind N Lumbhani ◽  
Nikunj J. Patel ◽  
...  
Keyword(s):  
Phosphoric Acid ◽  
Dosage Form ◽  
Potassium Dihydrogen Phosphate ◽  
Hplc Method ◽  
Simultaneous Estimation ◽  
Dihydrogen Phosphate ◽  
Potassium Dihydrogen ◽  
Rp Hplc ◽  
Tablet Dosage ◽  
Ich Guideline

A novel, simple, specific, accurate & precise stability-indicating Gradient reverse-phase high-performance liquid chromatography (RP-HPLC) method was developed for simultaneous estimation of Cilnidipine & Chlorthalidone in tablet dosage form, validated as per ICH guideline. The separation was achieved on Inertsil ODS column (250 mm x 4.6 mm, 5 μm) in a gradient mode.  The mobile phase consisted of Methanol, 0.025 M Potassium dihydrogen phosphate Buffer pH 5.5 adjusted by 10% v/v Ortho Phosphoric Acid (50:50 v/v) (Solution A) and Acetonitrile, 0.025 M Potassium dihydrogen phosphate Buffer pH 5.5 adjusted by 10%v/v Ortho Phosphoric Acid (75:25 v/v) (Solution B), gradient programming for 20 min at 1 ml/min rate of flow and response was detected at 225 nm. The retention time was found to be 3.580 min and 12.606 mins for Chlorthalidone and Cilnidipine, respectively. The method is validated according to ICH guideline, which includes linearity, specificity, accuracy, precision and robustness. Linearity was obtained over the concentration range of 10-60 μg/ml for Cilnidipine and 6.25-37.5 μg/ml for Chlorthalidone, had a regression coefficient (r2) almost 0.9966. The % Recovery was found to be 99.63-100.59 % and 100.24-100.51 % for Cilnidipine and Chlorthalidone, respectively. The method was found to be specific enough to separate all degradation products from the active compound. Drug samples were exposed to various stress conditions like photolysis, oxidation, heat conditions, and hydrolysis (acidic and alkaline), there was no interference of any degradants and excipient in the determination of drugs so that methods can be successfully applied for routine QC analysis.

Stability Indicating Assay Method Development and Validation of Simultaneous Estimation of Chlorzoxazone, Diclofenac Sodium and Paracetamol in Bulk Drug and Tablet by RP-HPLC

2021 ◽  
pp. 5024-5028
Author(s):  
Krutika Patel ◽  
Sudheer Kumar Verriboina ◽  
S.G. Vasantharaju
Keyword(s):  
Method Development ◽  
Diclofenac Sodium ◽  
Potassium Dihydrogen Phosphate ◽  
Hplc Method ◽  
Assay Method ◽  
Simultaneous Estimation ◽  
Dihydrogen Phosphate ◽  
Stability Indicating ◽  
Rp Hplc ◽  
Bulk Drug

A simple, accurate, specific and stability-indicating RP-HPLC method was developed for simultaneous determination of chlorzoxazone, diclofenac sodium and paracetamol, using C18 Vydac Monomeric 120A (250 × 4.6mm, 5μ) at 40ºC. The mobile phase contains a mixture of 20mM potassium dihydrogen phosphate buffer (pH 6.2 adjusted with potassium hydroxide) and acetonitrile (30:70 v/v). The flow rate was 1ml/min and detection was carried out at 275nm using PDA detector. The retention time of paracetamol, chlorzoxazone and diclofenac sodium were 3.28mins, 13.27mins and 15.61mins respectively. The analytical curve was linear over a concentration range of 0.65- 6.5μg/ml for paracetamol, 1-10μg/ml for chlorzoxazone and 0.1-1μg/ml for diclofenac sodium. The drugs in bulk and tablet were subjected to acid and alkali hydrolysis, oxidation, thermal and photolytic degradation. This method can be successfully employed for simultaneous quantitative analysis of Chlorzoxazone, Diclofenac sodium and Paracetamol in bulk drug and tablet formulation.

DEVELOPMENT OF LIQUID CHROMATOGRAPHIC METHOD FOR SIMULTANEOUS DETERMINATION OF BROMHEXINE HYDROCHLORIDE AND ENROFLOXACIN IN FORMULATIONS

INDIAN DRUGS ◽  
2018 ◽  
Vol 55 (02) ◽  
pp. 44-49
Author(s):  
P Choksi ◽  
◽  
F. Shaikh ◽  
D. A. Shah ◽  
K. Agarwal ◽  
...  
Keyword(s):  
Potassium Dihydrogen Phosphate ◽  
Fixed Dose ◽  
Dihydrogen Phosphate ◽  
Potassium Dihydrogen ◽  
Liquid Chromatographic Method ◽  
Dose Combination ◽  
Reproducible Method ◽  
Liquid Chromatographic ◽  
Isocratic Mode

A simple, specific, accurate, precise and reproducible method has been developed and validated for the estimation of bromhexine hydrochloride and enrofloxacin in fixed dose combination using RP-HPLC. The separation was achieved using stationary phase ODS Hypersil C18 column (250 mm× 4.6 mm i.d.) in isocratic mode, with mobile phase containing 0.05 M potassium dihydrogen phosphate buffer (pH 4 by o-phosphoric acid) : methanol: acetonitrile : triethylamine (40:20:40:01), at a flow rate of 1.0mL/min and eluents were monitored at 256 nm. The retention time of enrofloxacin and bromhexine HCl were found to be 3.00 min and 5.1 min respectively. The linearity for bromhexine HCl and enrofloxacin was in the range of 2-15 μg/mL and 20-150 μg/mL, respectively. The method was validated as per ICH guideline. The recoveries of bromhexine HCl and enrofloxacin were found in the range of 99.61-101.65% and 99.52-100.13 %, respectively. The method was successfully applied for the determination of both the drugs in combined dosage form.

scholarly journals Development and validation for determination of lisinopril dihydrate in bulk drug and formulation using RP-HPLC method

2018 ◽  
Vol 3 (2) ◽  
pp. 14-18
Author(s):  
Zahid Zaheer ◽  
Sarfaraz Khan ◽  
Mohammad Sadeque ◽  
Hundekari G. I. ◽  
Rana Zainuddin
Keyword(s):  
High Performance ◽  
High Performance Liquid Chromatographic ◽  
Hplc Method ◽  
Rp Hplc ◽  
Liquid Chromatographic Method ◽  
Bulk Drug ◽  
Development And Validation ◽  
Liquid Chromatographic ◽  
Isocratic Mode

A simple, reproducible and efficient reverse phase high performance liquid chromatographic method was developed for Lisinopril in bulk drug and formulation. A column having 150 × 4.6 mm in isocratic mode with mobile phase containing acetonitrile: phosphate buffer (70:30; adjusted to pH 3.0) was used. The flow rate was 0.8 ml/min and effluent was monitored at 216 nm. The retention time (min) and linearity range (μg/ml) for Lisinopril was (1.510) and (10-35). The developed method was found to be accurate, precise and selective for determination of Lisinopril in bulk and formulation.

Development and Validation of RP-HPLC Method for Simultaneous Estimation of Gatifloxacin and flurbiprofen Sodium in Eye Drops

2019 ◽  
Vol 9 (01) ◽  
pp. 83-88
Author(s):  
Pinkal Patel ◽  
Nalini Patel ◽  
Kinjal Parmar
Keyword(s):  
High Performance ◽  
Pharmaceutical Formulations ◽  
High Performance Liquid Chromatographic ◽  
Reversed Phase ◽  
Hplc Method ◽  
Simultaneous Estimation ◽  
Eye Drops ◽  
Rp Hplc ◽  
Development And Validation ◽  
Liquid Chromatographic

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.

Validated Chromatographic Methods for the Simultaneous Estimation of Etamsylate and Mefenamic Acid in the Presence of Their Main Impurities

2019 ◽  
Vol 15 (6) ◽  
pp. 624-631
Author(s):  
Asmaa Ahmed El-Zaher ◽  
Marianne Alphonse Mahrouse ◽  
Ahmed Mohammed Al-Ghani
Keyword(s):  
Quality Control ◽  
Mefenamic Acid ◽  
Potassium Dihydrogen Phosphate ◽  
Hplc Method ◽  
Routine Analysis ◽  
Simultaneous Estimation ◽  
Dihydrogen Phosphate ◽  
Chromatographic Methods ◽  
Rp Hplc ◽  
Ich Guidelines

Background: Etamsylate (ETS), a haemostatic drug, is formulated with mefenamic acid (MFA) for pain relief. Objective: The aim of this work was to develop chromatographic methods for the estimation of ETS and MFA in the presence of their main impurities. These methods could be used in the routine analysis in quality control laboratories. Methods: The first method was RP-HPLC method, the separation was carried out on an Inertsil® ODS- 3V C18 column using a mobile phase composed of acetonitrile: potassium dihydrogen phosphate buffer adjusted to pH 7 with 0.1 N NaOH (55: 45, v/v) at a flow rate of 1 ml/ min. The detection was carried out at 220 nm. The second method was a TLC-densitometric method where the studied components were separated using a developing system composed of dichloromethane: ethyl acetate: methanol: triethylamine (6: 2: 2: 0.5, v/v/v/v) on TLC silica gel 60 F254 plates, followed by densitometric scanning at 300 nm. Results: In RP-HPLC method, the peaks were sharp and well separated, good retention times were obtained. Linearity was obtained over the concentration range 20-90 µg/ml, for both ETS and MFA. In the TLC-densitometric method, well separation of drug spots and linear relationship were achieved over the concentration range of 0.4-2.8 µg/spot, for both ETS and MFA. Method validation was conducted according to ICH guidelines. Conclusion: The developed methods were applied for the determination of the cited drugs in laboratory prepared mixtures and in tablets containing the two drugs. The methods are simple and precise and can be used for routine analysis of the drugs in combined dosage forms in quality control laboratories.

scholarly journals A Versatile Liquid Chromatographic Method for the Simultaneous Determination of Metformin, Sitagliptin, Simvastatin, and Ezetimibe in Different Dosage Forms

2018 ◽  
Vol 101 (2) ◽  
pp. 401-409 ◽  
Author(s):  
Asmaa A El-Zaher ◽  
Ehab F Elkady ◽  
Hanan M Elwy ◽  
Mahmoud Abo El Makarim Saleh
Keyword(s):  
Potassium Dihydrogen Phosphate ◽  
Reversed Phase ◽  
Pharmaceutical Products ◽  
Metformin Hydrochloride ◽  
Dihydrogen Phosphate ◽  
Potassium Dihydrogen ◽  
Accuracy And Precision ◽  
Liquid Chromatographic Method ◽  
Liquid Chromatographic

Abstract A new LC method is introduced with the concept of its versatile application to widely used drugs from different pharmacological classes. Metformin hydrochloride (MTF), sitagliptin phosphate (SIT), simvastatin (SIM) and ezetimibe (EZB) were simultaneously determined with a simple reversed-phase LC method in which a SIT–SIM binary mixture, present in a dosage form brand, was considered central for its development. Chromatographic separation was achieved with a mobile phase of acetonitrile and 0.02 M potassium dihydrogen phosphate (pH 5.2) (77 + 23, v/v) flowing through a C18 column (BDS Hypersil, 250 × 4.6 mm, 5 µm) at 1.2 mL/min at ambient temperature. UV detection was programmed to be carried out at 210 nm for EZB, SIT, and MTF, whereas SIM was detected at 240 nm. The method was validated according to International Conference on Harmonization guidelines. Linearity, accuracy, and precision were satisfactory over concentration ranges 4–40 µg/mL for EZB and SIM, 0.5–50 µg/mL for SIT, and 5–500 µg/mL for MTF. Coefficients of determination were >0.99 for the four drugs. LOQs found were 0.01 µg/mL for EZB, 0.02 µg/mL for SIT, 0.2 µg/mL for MTF, and 0.02 µg/mL for SIM. The developed method is simple, rapid, accurate, precise, and suitable for the routine QC analysis of the cited drugs in pharmaceutical products by conventional HPLC systems.

scholarly journals Analytical method development and validation for simultaneous estimation of Fimasartan Potassium Trihydrate and Cilnidipine in synthetic mixture by HPLC for the treatment of hypertension stage-II

2021 ◽  
Vol 7 (1) ◽  
Author(s):  
Radhika G. Sojitra ◽  
Urvi J. Chotaliya
Keyword(s):  
Method Development ◽  
Potassium Dihydrogen Phosphate ◽  
Cost Effective ◽  
Hplc Method ◽  
Fixed Dose ◽  
Simultaneous Estimation ◽  
Dihydrogen Phosphate ◽  
Method Development And Validation ◽  
Dose Combination ◽  
Development And Validation

Abstract Background A specific, accurate, precise, robust, and cost-effective HPLC method was developed and validated for quantitative analysis of Fimasartan Potassium Trihydrate and Cilnidipine in fixed-dose combination. The isocratic elution was accomplished by Symmetry C18 column (150 mm × 4.6 mm, 5 µm) at 25 °C. Mobile phase composition is Methanol: Acetonitrile: Potassium Dihydrogen Phosphate buffer (pH 3) (60:05:35%v/v/v) at a flow rate of 1.0 mL/min, injection volume 20 µL with DAD detection at 240 nm. Result Fimasartan Potassium Trihydrate and Cilnidipine were eluted with retention time 2.65 min and 5.51 min respectively. This method was validated as per ICH guideline (Q2 R1). The calibration plots were over the concentration range of 15–90 μg/mL and 2.5–15 μg/mL for Fimasartan Potassium Trihydrate and Cilnidipine with correlation coefficient 0.9992 and 0.9989 respectively. Accuracy was obtained between 99.51–101.65% and 100.06–101.20% for Fimasartan Potassium Trihydrate and Cilnidipine respectively. LOD were found to be 0.97 μg/mL and 0.57 μg/mL and LOQ were found to be 2.95 μg/mL and 1.75 μg/mL for Fimasartan Potassium Trihydrate and Cilnidipine respectively. Conclusion The results showed that the developed method is reliable for the routine analysis for simultaneous determination of Fimasartan Potassium Trihydrate and Cilnidipine.

scholarly journals Development and Validation of RP-HPLC Method for the Simultaneous Estimation of Haloperidol and Trihexyphenidyl in API and Combined Tablet Dosage Form

2018 ◽  
Vol 3 (03) ◽  
pp. 36-40 ◽  
Author(s):  
E. Amulya ◽  
N. Naveen Kumar ◽  
CH. Mounika ◽  
V. Kowmudi ◽  
N. Supriya ◽  
...  
Keyword(s):  
High Performance ◽  
Dosage Form ◽  
Pharmaceutical Formulations ◽  
High Performance Liquid Chromatographic ◽  
Hplc Method ◽  
Simultaneous Estimation ◽  
Liquid Chromatographic Method ◽  
Development And Validation ◽  
Tablet Dosage ◽  
Liquid Chromatographic

A rapid and precise reverse phase high performance liquid chromatographic method has been developed for the validated of Trihexyphenidyl and Haloperidol, in its pure form as well as in tablet dosage form. Chromatography was carried out on a Altima C18 (4.6 x 150mm, 5μm) column using a mixture of Methanol: TEA Buffer pH 4.5: Acetonitrile (50:25:25) as the mobile phase at a flow rate of 1.0ml/min, the detection was carried out at 225 nm. The retention time of the Trihexyphenidyl and Haloperidol was 2.102, 3.537±0.02min respectively. The method produce linear responses in the concentration range of 15-75ppm of Trihexyphenidyland 37.5-187.5ppm of Haloperidol. The method precision for the determination of assay was below 2.0%RSD. The method is useful in the quality control of pharmaceutical formulations.

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