scholarly journals Development and Validation of a Simple and Selective Analytical HPLC Method for the Quantification of Oxaliplatin

2015 ◽  
Vol 2015 ◽  
pp. 1-6 ◽  
Author(s):  
Breno Noronha Matos ◽  
Paula Martins de Oliveira ◽  
Thaiene Avila Reis ◽  
Taís Gratieri ◽  
Marcílio Cunha-Filho ◽  
...  
Keyword(s):  
Future Development ◽  
Limit Of Detection ◽  
Hplc Method ◽  
Limit Of Quantification ◽  
Pharmaceutical Drug ◽  
Skin Cancers ◽  
Isocratic Hplc ◽  
Precision And Accuracy ◽  
Development And Validation ◽  
Analytical Hplc

Considering that currently published oxaliplatin (OXPt) analytical methods require complex procedures and equipment, the objective of this paper was to present the validation of a simple, rapid, precise, and specific isocratic HPLC method for quantification of OXPt. Such method will be essential during the future development of innovative, topical drug formulations for the treatment of mucosal and skin cancers. Validated method demonstrated OXPt separation without interference from the solvents or polymers with the most relevance for developing of bioadhesive pharmaceutical drug carries (chitosan and poloxamer). Method was linear(r>0.999)over studied OXPt concentration range (0.5–15.0 µg/mL) with acceptable precision and accuracy. Limit of detection (LOD) and limit of quantification (LOQ) were 0.099 µg/mL and 0.331 µg/mL, respectively.

scholarly journals DEVELOPMENT AND VALIDATION OF CARBAMAZEPINE PLASMA CONCENTRATIONS MEASUREMENT AND ITS APPLICATION ON EPILEPSY PATIENTS

2017 ◽  
Vol 9 (9) ◽  
pp. 87 ◽  
Author(s):  
Astri Budikayanti ◽  
Chiswyta Chaliana ◽  
Melva Louisa ◽  
Rianto Setiabudy
Keyword(s):  
Lower Limit ◽  
High Performance ◽  
Limit Of Detection ◽  
Plasma Concentrations ◽  
Internal Standard ◽  
Hplc Method ◽  
Limit Of Quantification ◽  
Relative Standard ◽  
Precision And Accuracy ◽  
Development And Validation

Objective: To develop and validate high-performance liquid chromatography with photodiode array (HPLC-PDA) detector as a method for measuring carbamazepine plasma concentrations in epilepsy patients treated with monotherapy or polytherapy.Methods: Carbamazepine was extracted from epilepsy patients’ plasma through liquid-liquid extraction, using protein precipitation with chloroform. Analysis was performed using HPLC with Inertsil DS-4 C18 (4.6x150 mm), 5 μm particle size column. The optimal condition for separation was established in a mobile phase consisting of acetonitrile: water (50:50) at a flow rate of 1.0 ml/min, detected by PDA detector at 220 nm. Propylparaben was used as the internal standard. The retention time was 3.5 min.Results: Linearity was obtained over a concentration range of 0.5-16 μg/ml with r = 0.999. The method showed good intra-and inter-day precision and accuracy of more than 90% difference (% diff) and 95% relative standard deviation (RSD). Lower limit of quantification (LOQ) was 0.5 μg/ml and lower limit of detection (LOD) was 0.2 μg/ml with 100% accuracy and more than 90% precision. Recovery test was nearly 100%. Stability of carbamazepine plasma concentration in 3 epilepsy patients was measured on the first and third month of treatment, ranging between 83.5 to 98.7%. When used to compare carbamazepine as a monotherapy versus polytherapy, the method showed good selectivity.Conclusion: The present HPLC method was valid for measuring carbamazepine plasma concentrations in epilepsy patients treated with monotherapy or polytherapy. This method meets the standard in the EMEA guideline in terms of linearity, precision, and accuracy, also selectivity in epilepsy patients treated with polytherapy.

scholarly journals Development and Validation of a Rapid RP-HPLC Method for the Estimation of Esmolol Hydrochloride in Bulk and Pharmaceutical Dosage Forms

2010 ◽  
Vol 7 (3) ◽  
pp. 807-812 ◽  
Author(s):  
Vanita Somasekhar ◽  
D. Gowri Sankar
Keyword(s):  
Limit Of Detection ◽  
Hplc Method ◽  
Detector Response ◽  
Reverse Phase Hplc ◽  
Limit Of Quantification ◽  
Pharmaceutical Dosage Forms ◽  
Rp Hplc ◽  
Accuracy And Precision ◽  
Development And Validation

A reverse phase HPLC method is described for the determination of esmolol hydrochloride in bulk and injections. Chromatography was carried on a C18column using a mixture of acetonitrile, 0.05 M sodium acetate buffer and glacial acetic acid (35:65:3 v/v/v) as the mobile phase at a flow rate of 1 mL/min with detection at 275 nm. The retention time of the drug was 4.76 min. The detector response was linear in the concentration of 1-50 μg/mL. The limit of detection and limit of quantification was 0.614 and 1.86 μg/mL respectively. The method was validated by determining its sensitivity, linearity, accuracy and precision. The proposed method is simple, economical, fast, accurate and precise and hence can be applied for routine quality control of esmolol hydrochloride in bulk and injections.

High performance liquid chromatography (HPLC) method development and validation for the determination of flunixin: Animal plasma based study

2021 ◽  
pp. 1-11
Author(s):  
Sultan M. Alshahrani ◽  
John Mark Christensen
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
High Performance ◽  
Method Development ◽  
Limit Of Detection ◽  
Hplc Method ◽  
Limit Of Quantification ◽  
Mobile Phases ◽  
Hplc Method Development ◽  
Development And Validation

This study was designed to develop and validate a simple and efficient high performance liquid chromatography (HPLC) method to determine flunixin concentrations in Asian elephant’s (Elephas maximus) plasma. Flunixin was administered orally at a dose of 0.8 mg/kg, and blood samples were collected. Flunixin extraction was performed by adding an equal amount of acetonitrile to plasma and centrifuging at 4500 rpm for 25 minutes. The supernatant was removed, and flunixin was analyzed using HPLC-UV detection. Two methods were developed and tested utilizing two different mobile phases either with or without adding methanol (ACN: H2O vs. ACN: H2O: MeOH). Both methods showed excellent linearity and reproducibility. The limit of detection was 0.05 ug/ml and limit of quantification was 0.1 ug/ml. the efficiency of flunixin recovery was maximized by the addition of methanol to mobile phase (ACN: H2O: MeOH as 50:30:20) at 95% in comparison to 23% without methanol. In conclusion, adding methanol to HPLC methods for extraction of flunixin from elephants’ plasma yielded higher recovery rate than without methanol.

METHOD DEVELOPMENT AND VALIDATION FOR THE SIMULTANEOUS ESTIMATION OF THYMOL AND EUGENOL BY USING RP-HPLC IN PURE AND IN EMULGEL FORMULATION

INDIAN DRUGS ◽  
2021 ◽  
Vol 58 (07) ◽  
pp. 59-65
Author(s):  
Vinita C. Patole ◽  
Shilpa P. Chaudhari ◽  
Keyword(s):  
High Performance ◽  
Method Development ◽  
Limit Of Detection ◽  
Hplc Method ◽  
Simultaneous Estimation ◽  
Limit Of Quantification ◽  
Relative Standard ◽  
Peak Areas ◽  
80 A 20 ◽  
Development And Validation

An attempt was made to develop a simple, selective, rapid and precise high-performance liquid chromatography (HPLC) method for simultaneous estimation of thymol and eugenol. Analysis was performed on a C18 column with the mobile phase consisting of solvent %A (water) and solvent %B (acetonitrile) with the following gradient: 0–1 min, 80 % A, 20 % B; 1–7 min, 40 % A and 60 % B; 7–12 min, 10 % A and 90 % B; and 12–15min, 80 % A and 20 % B at a flow rate of 0.6 mL/min. The compounds were well separated on a Thermo Scientific Hypersil BDS RP C18 column (4.6 mm × 150 mm, dp = 5 µm) and ultraviolet detection at 280 nm. The retention times of eugenol and thymol were 10.5 min and 11.6 min, respectively. Validation of the proposed method was carried out according to the guidelines of the International Council on Harmonization (ICH). The linearity of the method is good for thymol and eugenol over the concentration range of 1–50 ppm, and the r 2 values were 0.9996 for both thymol and eugenol. The calculated limit of detection (LOD) value was 0.5ppm and the limit of quantification (LOQ) value was 1ppm for both the analytes. The intra and interday relative standard deviation (RSD) of the retention time and peak areas was less than 3 %.The established method was appropriate, and the two markers were well resolved, enabling efficient quantitative analysis of thymol and eugenol.

scholarly journals Development and Validation of RP-Chiral HPLC Method for Determination of (R)-Enantiomer Excess Content in Efavirenz

2020 ◽  
Vol 32 (9) ◽  
pp. 2208-2212
Author(s):  
CH. RAMESH ◽  
DHARMASOTH RAMA DEVI DEVI ◽  
M.N.B. SRINIVAS ◽  
S. RADHA KRISHNA ◽  
NAGARAJU RAJANA ◽  
...  
Keyword(s):  
Limit Of Detection ◽  
Hplc Method ◽  
Chiral Hplc ◽  
Reverse Phase ◽  
Limit Of Quantification ◽  
Column Temperature ◽  
Enantiomer Excess ◽  
Development And Validation ◽  
Methyl Phenyl

simple, specific, linear, accurate and precise reverse phase chiral HPLC method was developed for the separation of efavirenz enantiomers by using the Lux Amylose-2 column containing amylose tris(5-chloro-2-methyl phenyl carbamate) as a stationary phase. The mobile phase consists of 0.1 % formic acid in water and acetonitrile (55:45, v/v). The flow rate was kept at 1.0 mL/min and the detection wavelength used 252 nm and the column temperature was set at 25 ºC. The limit of detection was 0.01 mg/mL and the limit of quantification was 0.04 mg/mL. The linearity calibration curve of (R)-enantiomer was shown well from the range of 0.04 mg/mL to 0.4 mg/mL. The values of the correlation coefficient were 0.999 and 0.999 for (R)-enantiomer and (S)-efavirenz, respectively. The percentage recoveries of (R)-enantiomer from efavirenz drug substance were ranged from 93.5% to 107.5%. The results demonstrated that developed RP-chiral HPLC method was simple, precise, robust and applicable for the estimation of (R)-enantiomer in efavirenz API. This method was validated in as per ICH Q2 (R1) and USP validation of compendial methods <1225>.

scholarly journals Research Article on Development and Validation of RP-HPLC Method for Estimation of Canagliflozin

2019 ◽  
Vol 11 (02) ◽  
pp. 85-92
Author(s):  
Gudipally. Mounika ◽  
K. Bhavya Sri ◽  
R. Swethasri ◽  
M. Sumakanth
Keyword(s):  
Retention Time ◽  
High Performance ◽  
Limit Of Detection ◽  
Hplc Method ◽  
Limit Of Quantification ◽  
Chromatography Method ◽  
Pharmaceutical Dosage Form ◽  
Validation Parameters ◽  
Liquid Chromatography Method ◽  
Development And Validation

To develop an accurate, precise, specific high performance liquid chromatography method for quantification of Canagliflozin in bulk and dosage forms. A C18 column (250mm X 4.6mm; 5μm phenomenex) was used with mobile phase containing Acetonitrile-0.1% sodium acetate buffer (pH-4.6), (20:80) in isocratic mode. The flow rate maintained was 1.0ml/min and the U.V detector was operated at 291nm. The retention time of Canagliflozin was 3.307min and showed a good linearity in concentration range of 2-14μg/ml with correlation coefficient of 0.999. The average percent recovery was found to be 99.98%. The developed method follows validation parameters such as system suitability, linearity, precision, accuracy, limit of detection and limit of quantification and robustness as per ICH guidelinesQ2(R1). The proposed method was found to provide faster retention time with sharp resolution with linearity at a lowest concentration as compared to previous methods and this method is validated as per International conference on harmonization guidelines and successfully applied for bulk and pharmaceutical dosage form.

DEVELOPMENT AND VALIDATION OF RP-HPLC METHOD FOR THE ESTIMATION OF LERCANIDIPINE IN BIOLOGICAL MATRICES

INDIAN DRUGS ◽  
2012 ◽  
Vol 49 (07) ◽  
pp. 49-53
Author(s):  
A Singla ◽  
◽  
Y. Paul ◽  
B. Singh
Keyword(s):  
Limit Of Detection ◽  
Quantitative Estimation ◽  
Reversed Phase ◽  
Hplc Method ◽  
Biological Matrices ◽  
Limit Of Quantification ◽  
Rp Hplc ◽  
Uv Visible ◽  
Development And Validation ◽  
Isocratic Mode

A simple, precise, accurate, reproducible and robust analytical method was developed using reversed phase HPLC for quantitative estimation of lercanidipine in biological matrices. The method was validated as per the ICH and FDA guidelines. Analysis of the drug was performed in an isocratic mode employing methanol and acetonitrile (74:26) as the mobile phase on a C18 column. UV-Visible detector at 219 nm was found to be suitable for drug estimation. Linearity was observed in the range of 5 and 500 ng/mL (p<0.001). Recovery was found to range between 96.26% and 100.67%. The % RSD values for method precision and system precision were found to be 0.437 and 1.58, respectively. Limit of detection (LOD) and limit of quantification (LOQ) were observed to be 0.20 ng/mL and 0.68 ng/mL, respectively.

Development and Validation of Novel GC-FID Method for Simultaneous Quantification of Paracetamol and Caffeine in Formulations

2020 ◽  
Vol 42 (4) ◽  
pp. 581-581
Author(s):  
Imtiaz Hussain Imtiaz Hussain ◽  
Yawar Baig Yawar Baig ◽  
Sara Naveed Sara Naveed ◽  
Muhammad Imran Khan Muhammad Imran Khan ◽  
Hafiz Shoaib Sarwar Hafiz Shoaib Sarwar ◽  
...  
Keyword(s):  
Limit Of Detection ◽  
Analytical Techniques ◽  
Hplc Method ◽  
Limit Of Quantification ◽  
Simultaneous Quantification ◽  
Ich Guidelines ◽  
Highly Sensitive ◽  
Sensitivity And Selectivity ◽  
Development And Validation ◽  
Accurate Quantification

The advancements in analytical techniques have enabled the development of highly sensitive and accurate methods for the identification of materials up to trace levels using microliter of sample. A highly sensitive and novel GC-FID method has been developed and reported herein for the simultaneous quantification of paracetamol (PCM) and caffeine (CAF) in samples up to trace levels. The method was validated as per ICH guidelines for its sensitivity, linearity, robustness, inter and intra-day variations, limit of quantification (LOQ), limit of detection (LOD), matrix effect, carryover, precision, and accuracy. The LOD of PCM and CAF were determined to be 100 ppm and 10 ppm whereas, LOQ of PCM and CAF were found to be 300 and 30 ppm respectively. The method was applied to quantify PCM and CAF in marketed tablets and dissolution samples of the tablets, which showed highly precise and accurate quantification of PCM and CAF. Moreover, the GC-FID method was compared with reported HPLC method which suggested the superiority of GC-FID method in performance and sensitivity. In short, the newly developed GC-FID method showed sensitivity and selectivity for PCM and CAF estimation and can be adopted as an efficient method for various applications.

DEVELOPMENT AND VALIDATION OF RP HPLC METHOD FOR THE ESTIMATION OF SOFOSBUVIR IN BULK, TABLET AND INDUSTRIAL WASTE WATER

INDIAN DRUGS ◽  
2019 ◽  
Vol 56 (06) ◽  
pp. 59-66
Author(s):  
V Dhanunjayachary ◽  
◽  
V.L.S. Likhitha ◽  
Sri K. Vijaya ◽  
M. A Madhuri
Keyword(s):  
Industrial Waste ◽  
Limit Of Detection ◽  
Hplc Method ◽  
Limit Of Quantification ◽  
Pharmaceutical Dosage Form ◽  
Rp Hplc ◽  
Ich Guidelines ◽  
System Suitability ◽  
Limit Of Quantitation ◽  
Development And Validation

The study was aimed at development and validation of RP-HPLC method for estimation of sofosbuvir in bulk, pharmaceutical dosage form and pharmaceutical industrial waste. The chromatographic separation was performed on Agilent Syncronis C 18 (100 mm × 4.6 mm, 5μm) column, with a mobile phase comprising of a mixture of methanol: acetonitrile: water (45:30:25 v/v/V). The flow rate was 1.0 mL/min with detection at 260 nm. Retention time of sofosbuvir was found to be 2.040 min. As per ICH guidelines, the method was validated for linearity, accuracy, limit of detection, limit of quantitation, precision, robustness and system suitability. Linearity was found to be in the range of 4-24 μg/mL with regression equation y = 675284.x + 49120 and correlation coefficient 0.999. The low % RSD values indicate the method to be accurate and precise. The limit of detection (LOD) and limit of quantification (LOQ) were found to be 0.046 and 0.1400 μg/mL, respectively. The % recovery of tablets was found to be in the range of 99.9– 101.3%. It can be concluded that this validated HPLC method is easy, precise, accurate, sensitive and selective for estimation of sofosbuvir in bulk, tablet and applicable for analyses of in pharmaceutical industrial waste.

scholarly journals DEVELOPMENT AND VALIDATION OF STABILITY INDICATING METHOD RP-HPLC METHOD OF ACOTIAMIDE

2018 ◽  
Vol 10 (9) ◽  
pp. 1 ◽  
Author(s):  
Charu P. Pandya ◽  
Sadhana J. Rajput
Keyword(s):  
Limit Of Detection ◽  
Hplc Method ◽  
Limit Of Quantification ◽  
Stability Indicating ◽  
Stability Indicating Method ◽  
Rp Hplc ◽  
Acid And Base ◽  
Stress Degradation ◽  
Development And Validation ◽  
Tablet Dosage

Objective: The objective of present work was to develop and validate simple, precise, accurate and specific stability indicating method for determination of acotiamide in presence of its degradation products.Methods: An isocratic RP-HPLC method has been developed using C-8 Thermo Hypersil BDS Column (250 x 4.6 mm i.d., 5µparticle size) with the mobile phase composition of acetonitrile: 0.1 % triethylamine in 0.2% formic acid (30: 70) at column oven temperature of 40 °C. The flow rate was 1.0 ml min-1 and effluent was detected at 282 nm. The method was validated in terms of linearity, accuracy, precision, LOD (Limit of Detection), LOQ (Limit of Quantification) and robustness as per ICH guidelines.Results: The method was found to be linear in the range of 10-60µg/ml. Limit of detection and limit of quantification was found to 0.36µg/ml and 1.10 µg/ml.% Recovery was found to be in the range of 99.45%-99.75%and precision less than 2%. The developed method was successfully applied for estimation of Acotiamide in marketed tablet formulation and percentage assay was found to be 100.45%. Acotiamide was subjected to stress degradation under acid, base, neutral hydrolysis, oxidation, dry heat, photolysis conditions. Significant degradation was observed in acid and base degradation.Conclusion: The developed RP-HPLC method was simple, rapid, accurate, precise and stability indicating for the estimation of Acotiamide in bulk and tablet dosage form.

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