A simple reverse phase UPLC validated method for concurrent estimation of Emtricitabine, Darunavir, Tenofovir and Cobicistat in drug substances and drug product

2021 ◽  
Vol 25 (9) ◽  
pp. 79-88
Author(s):  
Suresh Gandi ◽  
Manikandan Ayyar ◽  
Venkat Rao Sirugubattula
Keyword(s):  
Flow Rate ◽  
Mobile Phase ◽  
Drug Product ◽  
Chromatographic Technique ◽  
Reverse Phase ◽  
Drug Substances ◽  
Liquid Chromatographic ◽  
Concurrent Estimation

A fast, precise, accurate and steady isocratic liquid chromatographic technique was created for the synchronous assurance of the Emtricitabine, Darunavir, Tenofovir and Cobicistat in bulk and in formulation. To optimize a column HSS C18 100 x 2.1 mm, 1.8mm, mobile phase including Buffer 0.01N KH2PO4(5.4pH): Acetonitrile pick in the proportion 60:40v/v was pumped through column at a flow rate of 0.3 ml/min at 260nm. The retention times of Emtricitabine, Darunavir, Tenofovir and Cobicistat were initiated to be 1.066 min, 1.727 min, 2.574 min and 2.977 min. % recovery was 99.75%, 100.05%, 100.42% and 100.59% for Emtricitabine, Darunavir, Tenofovir and Cobicistat respectively. LOD and LOQ values got from relapse formula of Emtricitabine, Darunavir, Tenofovir and Cobicistat and were 0.18, 0.54, 0.71,2.14, 0.01,0.05 0.44 and 1.32 correspondingly. Relapse equation of Emtricitabine is y = 13375x + 2577.4, for Darunavir it is y = 7196.3x + 2981.2, for Tenofovir it is y = 66663x + 1338.9 and y = 22723x + 6978.7 for Cobicistat.

scholarly journals A Simple Reverse Phase Ultra Performance Liquid Chromatography Validated Method for Concurrent Estimation of Daunorubicin and Cytarabine in Drug Substances and Drug Product

2020 ◽  
Vol 11 (03) ◽  
pp. 424-429
Author(s):  
Suresh Gandi ◽  
Manikandan Ayyar ◽  
Venkat Rao Sirugubattula ◽  
Murali Krishna Cheepi
Keyword(s):  
Orthophosphoric Acid ◽  
Limit Of Detection ◽  
Drug Product ◽  
Ultra Performance Liquid Chromatography ◽  
Chromatographic Technique ◽  
Reverse Phase ◽  
Drug Substances ◽  
Limit Of Quantitation ◽  
Liquid Chromatographic ◽  
Concurrent Estimation

A fast, precise, accurate, and steadiness indicating isocratic liquid chromatographic technique was created for the synchronous assurance of the daunorubicin and cytarabine in bulk and formulation. To optimize a column CHS C18 100 × 2.1 mm, 1.8 μm, mobile phase, including buffer 0.1% orthophosphoric acid, acetonitrile pick in the proportion 70:30 v/v, was pumped through the column at a flow rate of 0.3 mL/min at 240 nm, initiate to be an efficient method for elution of drug with good peak shapes, as well as, retention times. The retention time of daunorubicin and cytarabine were initiated to be 0.556 and 0.743 minutes. The % recovery was got at 100.07 and 99.88% for daunorubicin and cytarabine separately. The limit of detection (LoD) and limit of quantitation (LoQ) values got from the relapse formula of daunorubicin and cytarabine were 0.16, 0.5, and 0.64, 1.93, correspondingly. The relapse equation of daunorubicin is y = 2974.3x + 648.32, and y = 4896.5x + 4851.5 of cytarabine.

Development, Validation and Application of HPLC Method for Metformin in Rabbit Plasma

2019 ◽  
Vol 15 (6) ◽  
pp. 574-579
Author(s):  
Muhammad Ubaid ◽  
Mahmood Ahmad ◽  
Farhan Ahmad Khan ◽  
Ghulam Murtaza
Keyword(s):  
Flow Rate ◽  
Present Method ◽  
Mobile Phase ◽  
Hplc Method ◽  
Plasma Samples ◽  
Rabbit Plasma ◽  
Uv Detector ◽  
Reverse Phase ◽  
T Values ◽  
Pharmacokinetic Evaluation

Objective:This study was aimed at conducting a pharmacokinetic evaluation of metformin in rabbit plasma samples using rapid and sensitive HPLC method and UV detection.Methods:Acetonitrile was used for protein precipitation in the preparation of plasma samples. Reverse phase chromatography technique with silica gel column (250 mm × 4.6 mm, 5 μm) at 30°was used for the separation purpose. Methanol and phosphate buffer (pH 3.2) mixture was used as a mobile phase with flow rate 0.8 ml/min. The wavelength of UV detector was adjusted at 240 nm.Results:The calibration curve was linear in a range of 0.1-1 µg/ml with R² = 0.9982. The precision (RSD, %) values were less than 2%, whereas, accuracy of method was higher than 92.37 %. The percentage recovery values ranged between 90.14 % and 94.97 %. LOD and LOQ values were 25 ng/ml and 60 ng/ml, respectively. Cmax and AUC0-t values were found to be 1154.67 ± 243.37 ng/ml and 7281.83 ± 210.84 ng/ml.h, respectively after treating rabbits with a formulation containing 250 mg metformin.Conclusion:Based on the above findings, it can be concluded that present method is simple, precise, rapid, accurate and specific and thus, can be efficiently used for the pharmacokinetic study of metformin.

scholarly journals RP-HPLC Determination of Raloxifene in Pharmaceuticl Tablets

2006 ◽  
Vol 3 (1) ◽  
pp. 60-64 ◽  
Author(s):  
P. Venkata Reddy ◽  
B. Sudha Rani ◽  
G. Srinu Babu ◽  
J. V. L. N. Seshagiri Rao
Keyword(s):  
Flow Rate ◽  
Retention Time ◽  
Mobile Phase ◽  
Dosage Forms ◽  
Hplc Method ◽  
Reverse Phase Hplc ◽  
Reverse Phase ◽  
Pharmaceutical Dosage Forms ◽  
Rp Hplc

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.

QUALITY BY DESIGN APPROACH (QBD) FOR THE SIMULTANEOUS ESTIMATION OF CANDESARTAN CILEXETIL AND AMLODIPINE BESYLATE BY RP–HPLC

INDIAN DRUGS ◽  
2020 ◽  
Vol 57 (08) ◽  
pp. 41-52
Author(s):  
Ankita Kamli ◽  
Megha Shah ◽  
Madhuri Hinge
Keyword(s):  
Experimental Design ◽  
Flow Rate ◽  
Quality By Design ◽  
Candesartan Cilexetil ◽  
Design Approach ◽  
Simultaneous Estimation ◽  
Chromatographic Technique ◽  
Amlodipine Besylate ◽  
Quality By Design Approach ◽  
Liquid Chromatographic

A revers phase liquid chromatographic technique has been developed for the separation and determination of candesartan cilexetil and amlodipine besylate using QbD (Quality by Design) approach. The present method was optimised by introducing experimental design approach to identify the chromatographic conditions for adequate separation quality and minimal analysis duration. The relation between independent variables and critical quality attributes is given by experimental design methodology. The separation was achieved on shim-pack solar C18 type column (250 mm × 4.6 mm, 5 µm) as stationary phase; acetonitrile: phosphate buffer pH 6.8 (82:18, v/v); 1.0 ml/min as flow rate; detection wavelength 235 nm. The chromatographic efficiency was investigated for the factorial effect of percentage organic phase and flow rate and finely optimized by employing factorial design experiment. The method was validated and was found to be accurate, precise and robust.

Liquid Chromatographic Determination of Carbofuran in Technical and Formulated Products: Collaborative Study

1986 ◽  
Vol 69 (5) ◽  
pp. 915-918
Author(s):  
Edward J Kikta ◽  
◽  
E Bane ◽  
A Burns ◽  
A Christensen ◽  
...  
Keyword(s):  
Mobile Phase ◽  
Collaborative Study ◽  
Internal Standard ◽  
Chromatographic Determination ◽  
Data Sets ◽  
Matched Pairs ◽  
Reverse Phase ◽  
Liquid Chromatographic Determination ◽  
Liquid Chromatographic

Abstract A liquid chromatographic (LC) method for the analysis of technical and formulated carbofuran samples was evaluated in a collaborative study. Carbofuran is determined by reverse phase LC, using a water-methanol mobile phase and acetophenone as internal standard, and detected at 280 nm. Twelve samples, 5 formulations and technical matched pairs, were analyzed by 17 collaborating laboratories. Accuracy and variability of results are typical of large LC data sets. The method has been adopted official first action.

Reverse Phase Liquid Chromatographic Determination of Dexamethasone Acetate and Cortisone Acetate in Bulk Drug Substances and Dosage Forms: Method Development

1987 ◽  
Vol 70 (5) ◽  
pp. 829-833
Author(s):  
Linda L Ng
Keyword(s):  
Mobile Phase ◽  
Method Development ◽  
Chromatographic Determination ◽  
Dosage Forms ◽  
Cortisone Acetate ◽  
Drug Substances ◽  
Dexamethasone Acetate ◽  
Bulk Drug ◽  
Liquid Chromatographic

Abstract The determination of the steroid acetates was evaluated for ruggedness of the method by using an octyldecylsilane column, 254 nm detection, and acetonitrile-water as mobile phase. Mobile phase pH, oven temperature, and columns from various manufacturers had no dramatic effect on the chromatography. The method was then optimized for dexamethasone acetate and cortisone acetate bulk drug and dosage forms. For dexamethasone acetate, the bulk drug substance should be dried at 105°C before use, and the sample should be dissolved in 50% acetonitrile-buffer pH 6 for stability. Cortisone acetate, on the other hand, was found to be nonhygroscopic and hence could be used as received. For stability, the sample should be stored in 50% acetonitrile-buffer pH 4

scholarly journals Quantitation of Sitagliptin in Drug Product by Validated Reversed Phase Liquid Chromatographic Technique

2018 ◽  
Vol 17 (1) ◽  
pp. 123-129
Author(s):  
Sharifa Sultana ◽  
Md Shahadat Hossain ◽  
Md Samiul Islam ◽  
Abu Shara Shamsur Rouf
Keyword(s):  
High Performance ◽  
Drug Product ◽  
Linear Regression Analysis ◽  
Analysis Data ◽  
High Performance Liquid Chromatographic ◽  
Reversed Phase ◽  
Chromatographic Technique ◽  
Pharmaceutical Dosage Form ◽  
Relative Standard ◽  
Liquid Chromatographic

A novel reversed phase ultra-high performance liquid chromatographic (RP-UHPLC) method was developed for the estimation of sitagliptin in pharmaceutical dosage form. Separation was done by a X-bridge C18 column (4.6 i.d.× 150 mm, 5 μm particle size) with a flow rate of 1 ml/min using phosphate buffer (pH 6) and acetonitrile (70:30, v/v) as mobile phase at 268 nm using photodiode array plus (PDA+) detector. The retention time was found at 4.607 min. The developed method was validated as per the requirements of ICH-Q2B guidelines for specificity, system suitability, linearity, precision, accuracy, sensitivity and robustness. The linear regression analysis data for the linearity plot showed correlation coefficient values of 0.999 with LOD value of 0.06 μg/ml and LOQ of 0.225 μg/ml. The relative standard deviation (%RSD) for inter-day and intra- day precision was not more than 2.0%. The method was found to be accurate with percentages recovery of 98.50±0.03 to 99.70±0.05 and the % RSD was less than 2. The results showed that the proposed method is highly convenient for routine analysis of sitagliptin.Dhaka Univ. J. Pharm. Sci. 17(1): 123-129, 2018 (June)

scholarly journals HPLC Method for Determination of Aspirin, Rosuvastatin, Ezetimibe and Clopidogrel in Combination Drug Products

2019 ◽  
Vol 31 (10) ◽  
pp. 2275-2283 ◽  
Author(s):  
Suresh Kumar Palacharla ◽  
G.V. Krishna Mohan
Keyword(s):  
Method Validation ◽  
Flow Rate ◽  
Mobile Phase ◽  
Drug Product ◽  
Hplc Method ◽  
Combination Drug ◽  
Injection Volume ◽  
Drug Products ◽  
Product Manufacturing

A single HPLC method for the determination of four active ingredients viz. aspirin, rosuvastatin, ezetimibe and clopidogrel in less run time is developed. HPLC method was developed and validated. X-terra C18 100 × 4.6 mm, 3.5 μ HPLC column, KH2PO4 buffer (mobile phase A) and acetonitrile (mobile phase B) were used. 20 μ injection volume, 1.0 mL/min flow rate, 230 nm and ambient column oven temperature were applied for separation. Gradient program: at 0 min mobile phase-B 13 %, at 4 min 13 %, at 8 min 44 %, 14 min 57 %, 17 min 57 %, 20 min 13 % and 25 min 13 %. Method validation was performed as per ICH guidance with precision, linearity, specificity, accuracy, ruggedness and robustness. Validation results were satisfactory and this method can be applied for regular drug product manufacturing

Simultaneous very fast liquid-chromatographic analysis of ethosuximide, primidone, phenobarbital, phenytoin, and carbamazepine in serum.

1983 ◽  
Vol 29 (3) ◽  
pp. 473-476 ◽  
Author(s):  
P M Kabra ◽  
M A Nelson ◽  
L J Marton
Keyword(s):  
Particle Size ◽  
Flow Rate ◽  
Chromatographic Analysis ◽  
Mobile Phase ◽  
Internal Standard ◽  
Reversed Phase ◽  
Ultraviolet Detector ◽  
Analytical Recovery ◽  
Liquid Chromatographic Analysis ◽  
Liquid Chromatographic

Abstract We describe a sensitive, specific, and very fast liquid-chromatographic assay for simultaneously determining five anticonvulsants (ethosuximide, primidone, phenobarbital, phenytoin, and carbamazepine) by using commercially available 5- or 3-microns particle size reversed-phase columns and a microflow-cell-equipped ultraviolet detector. The anticonvulsant drugs are extracted from 200 microL of serum containing 50 mg of cyclopal per liter as an internal standard, by elution from a Bond-Elut (Analytichem International, Harbor City, CA 90710) column with 300 microL of methanol. A 5-microL aliquot of the eluate is applied to an analytical column and eluted with a mobile phase of acetonitrile/methanol/phosphate buffer, 20 mmol/L, pH 3.7 (13.5/35/51.5 by vol), at a flow rate of 3.0 mL/min and at 50 degrees C. Detection is at 210 or 195 nm. The chromatography is complete in less than 2.5 min with the 5-microns-particle column, and in less than 1.4 min with the 3-microns-particle column. The sensitivity of the method for all drugs is less than 1 mg/L. Analytical recovery of drugs added to serum ranged from 92 to 109% for concentrations up to 200 mg/L. Between-run precision (CV) ranged from 1.3 to 4.1%.

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