Development and Validation of HPLC/UV-Spectrophotometric Procedures for Metronidazole Quantitative Determination

2018 ◽  
Vol 9 (3) ◽  
Author(s):  
Klimenko Lina Yu ◽  
Shkarlat Galyna L ◽  
Shovkova Zoia V ◽  
Yaremenko Vitaliy D ◽  
Shpychak Oleg S
Keyword(s):  
Quantitative Determination ◽  
Sodium Hydroxide Solution ◽  
Gradient Elution ◽  
Calibration Model ◽  
Column Temperature ◽  
Medical Laboratories ◽  
Accuracy And Precision ◽  
Development And Validation ◽  
Gradient Elution Mode ◽  
Potential Object

Metronidazole is the most popular representative of antiprotozoal medicines from the group of 5-nitroimidazoles. Metronidazole blocks the enzymes of alcohol dehydrogenase and acetaldehyde dehydrogenase, therefore when its joint taking with alcohol it is observed the strong intoxication syndrome and fatal poisonings too. Therefore metronidazole can be a potential object of chemical toxicological investigations. The purpose of our paper is to develop HPLC/UV-procedure of metronidazole quantification with application of the system of HPLC-analyzer MiLiChrome® A-0230 implemented in practice of forensic medical laboratories in Russia and Ukraine and carry out step-by-step validation of the developed procedure. Chromatographic conditions: Eluent A (0.2 M LiClO4 – 0.005 M HClO4) and Eluent B (acetonitrile) wereused as the mobile phase components; HPLC microcolumn Ø2×75 mm and ProntoSIL 120-5-C18 AQ, 5 μm were used as an analytical column; temperature was 40°С; flow rate was 100 μl/min; gradient elution mode was from 5% to 100% Eluent B for 40 min, then 100% Eluent B for 3 min; detection was performed at 277 nm. Retention time for metronidazole is 5.95 min. Since metronidazole is easy soluble and stable enough in the solutions of diluted alkalis 0.001 M sodium hydroxide solution has been proposed for preparation of the solutions in developing HPLC/UV-procedure of metronidazole quantification. Validation of the procedure has been carried out in the variants of the method of calibration curve and method of standard by such parameters as in process stability, linearity/calibration model, accuracy and precision within 3 different analytical runs using different batches of reagents and different glassware; experiments have been performed by three different analysts. New procedure of metronidazole quantitative determination by the method of HPLC/UV has been developed. Its validation has been carried out and acceptability for application has been shown.

scholarly journals Simultaneous and Trace Level Determination of Six Potential Impurities by UPLC-ESI-MS/MS in Antiarrhythmic Drug: Dronedarone Hydrochloride

2020 ◽  
Vol 32 (5) ◽  
pp. 1183-1190
Author(s):  
K. Durga Raja ◽  
V. Saradhi Venkata Ramana ◽  
K. Raghu Babu ◽  
B. Kishore Babu ◽  
V. Jagadeesh Kumar ◽  
...  
Keyword(s):  
Mobile Phase ◽  
Gradient Elution ◽  
Ultra Performance Liquid Chromatography ◽  
Solvent Mixture ◽  
Column Temperature ◽  
Esi Ms ◽  
Quantitation Limit ◽  
Ich Guidelines ◽  
Validation Tests ◽  
Development And Validation

Development and validation of six potential impurities by ultra performance liquid chromatography electro spray ionization tandem mass (UPLC-ESI-MS/MS) method for dronedarone hydrochloride drug was accomplished coherent with ICH guidelines. Successful chromatographic separation of dronedarone with its six impurities was attained by using gradient elution mode on RP-UPLC column using three pump mode system of 0.1 % formic acid in water as mobile phase A, methanol as the mobile phase B and solvent mixture of methanol, acetonitrile and water in the ratio of 65:30:5 v/v/v as the mobile phase C. Chromatographic conditions were set as 0.3 mL min-1 flow rate at the column temperature of 45 °C with the injection volume 2 μL. Briefly, the method enabled quantitation of six impurities with high accuracy (recovery > 90 %) and precision (% RSD < 5.0),within the ranges of 0.18-2.82 μg g-1. The regression (r) for each impurity over a range was > 0.99. The detection limit and quantitation limit of impurities were set at 0.09 and 0.18 μg g-1, respectively. The performed validation tests proved the suitability of the method for its intended purposes.

Development and Validation of UV-spectrophotometric Procedures for Efavirenz Quantitative Determination

2018 ◽  
Vol 9 (3) ◽  
Author(s):  
Klimenko Lina Yu ◽  
Slabiak Oksana I ◽  
Ivanchuk Iryna M ◽  
Tokaryk Galyna V ◽  
Kolisnyk Iuliia S
Keyword(s):  
Quantitative Determination ◽  
Sodium Hydroxide ◽  
Sodium Hydroxide Solution ◽  
Transcriptase Inhibitor ◽  
Uv Spectra ◽  
Uv Spectrophotometry ◽  
High Concentration ◽  
Hydroxide Solution ◽  
Development And Validation ◽  
Accuracy And Repeatability

Efavirenz is a non-nucleoside reverse transcriptase inhibitor and attributed to the group of antiretroviral medicines used for treatment of HIV infection. For efavirenz determination the method of HPLC is widely used, but efavirenz is applied in high concentration and less sensitive methods of analysis such as spectrophotometry may be useful for its quantification. The aim is to develop UV-spectrophotometric procedures of efavirenz quantification and carry out step-by-step validation of the developed procedures. UV-spectra of efavirenz in 96% ethanol and 0.1 M sodium hydroxide solution have been investigated and the absorption maximums are observed at 247 nm and 267 nm respectively. The procedures of efavirenz quantitative determination by the method of UV-spectrophotometry have been developed using the mentioned solvents and wavelengths respectively. Their validation by such parameters as stability, linearity, accuracy and precision in the variants of the method of calibration curve, method of standard and method of additions has been carried out. All procedures of efavirenz quantitative determination are acceptable for application. The best linearity, accuracy and repeatability have been fixed for the procedure with application of 0.1 M sodium hydroxide solution as a solvent in the variant of the method of additions.

Development and Validation of the Chiral HPLC Method for Daclatasvir in Gradient Elution Mode on Amylose-Based Immobilized Chiral Stationary Phase

2016 ◽  
Vol 79 (21-22) ◽  
pp. 1457-1467 ◽  
Author(s):  
G. Srinivasu ◽  
K. Nagesh Kumar ◽  
Ch. Thirupathi ◽  
Ch. Lakshmi Narayana ◽  
Ch. Parameswara Murthy
Keyword(s):  
Stationary Phase ◽  
Chiral Stationary Phase ◽  
Gradient Elution ◽  
Hplc Method ◽  
Chiral Hplc ◽  
Development And Validation ◽  
Gradient Elution Mode

scholarly journals Analytical quality by design methodology for botanical raw material analysis: a case study of flavonoids in Genkwa Flos

2021 ◽  
Vol 11 (1) ◽  
Author(s):  
Min Kyoung Kim ◽  
Sang Cheol Park ◽  
Geonha Park ◽  
Eunjung Choi ◽  
Yura Ji ◽  
...  
Keyword(s):  
High Performance ◽  
Quality By Design ◽  
Analytical Data ◽  
Gradient Elution ◽  
Raw Material ◽  
Analytical Quality ◽  
Factor Screening ◽  
Column Temperature ◽  
Relative Standard ◽  
Critical Method

AbstractThe present study introduces a systematic approach using analytical quality by design (AQbD) methodology for the development of a qualified liquid chromatographic analytical method, which is a challenge in herbal medicinal products due to the intrinsic complex components of botanical sources. The ultra-high-performance liquid chromatography-photodiode array-mass spectrometry (UHPLC-PDA-MS) technique for 11 flavonoids in Genkwa Flos was utilized through the entire analytical processes, from the risk assessment study to the factor screening test, and finally in method optimization employing central composite design (CCD). In this approach, column temperature and mobile solvent slope were found to be critical method parameters (CMPs) and each of the eleven flavonoid peaks’ resolution values were used as critical method attributes (CMAs) through data mining conversion formulas. An optimum chromatographic method in the design space was calculated by mathematical and response surface methodology (RSM). The established chromatographic condition is as follows: acetonitrile and 0.1% formic acid gradient elution (0–13 min, 10–45%; 13–13.5 min, 45–100%; 13.5–14 min, 100–10%; 14–15 min, 10% acetonitrile), column temperature 28℃, detection wavelength 335 nm, and flow rate 0.35 mL/min using C18 (50 × 2.1 mm, 1.7 μm) column. A validation study was also performed successfully for apigenin 7-O-glucuronide, apigenin, and genkwanin. A few important validation results were as follows: linearity over 0.999 coefficient of correlation, detection limit of 2.87–22.41, quantitation limit of 8.70–67.92, relative standard deviation of precision less than 0.22%, and accuracy between 100.13 and 102.49% for apigenin, genkwanin, and apigenin 7-O-glucuronide. In conclusion, the present design-based approach provide a systematic platform that can be effectively applied to ensure pharmaceutically qualified analytical data from complex natural products based botanical drug.

scholarly journals Determination of Triterpenoids and Phenolic Acids from Sanguisorba officinalis L. by HPLC-ELSD and Its Application

Molecules ◽  
2021 ◽  
Vol 26 (15) ◽  
pp. 4505
Author(s):  
Jiahui Sun ◽  
Chunli Gan ◽  
Jing Huang ◽  
Zhenyue Wang ◽  
Chengcui Wu ◽  
...  
Keyword(s):  
Phenolic Acids ◽  
High Performance ◽  
Gradient Elution ◽  
Light Scattering Detection ◽  
Evaporative Light Scattering ◽  
Acetic Acid Water ◽  
Sanguisorba Officinalis ◽  
Functional Components ◽  
Gradient Elution Mode

A novel analytical method involving high-performance liquid chromatography with evaporative light scattering detection (HPLC-ELSD) was developed for simultaneous determination of 11 phenolic acids and 12 triterpenes in Sanguisorba officinalis L. Chromatographic separation was conducted with gradient elution mode by using a DiamonsilTM C18 column (250 mm × 4.6 mm, 5 μm) with the mobile phase of 0.1% acetic acid water (A) and methanol (B). The drift tube temperature of ELSD was set at 70 °C and the nitrogen cumulative flow rate was 1.6 L/min. The method was fully validated to be linear over a wide concentration range (R2 ≥ 0.9991). The precisions (RSD) were less than 3.0% and the recoveries were between 97.7% and 101.4% for all compounds. The results indicated that this method is accurate and effective for the determination of 23 functional components in Sanguisorba officinalis L. and could also be successfully applied to study the influence of processing method on those functional components in Sanguisorba officinalis L.

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.

scholarly journals Development and Validation of UV Spectrophotometric Method for the Determination of Cefuroxime Axetil in Bulk and Pharmaceutical Formulation

2013 ◽  
Vol 6 (1) ◽  
pp. 133-141 ◽  
Author(s):  
S. Binte Amir ◽  
M. A. Hossain ◽  
M. A. Mazid
Keyword(s):  
Spectrophotometric Method ◽  
Cost Effective ◽  
Cefuroxime Axetil ◽  
Pharmaceutical Formulation ◽  
Uv Spectrum ◽  
Accuracy And Precision ◽  
Relative Standard ◽  
Label Claim ◽  
Development And Validation

The present study was undertaken to develop and validate a simple, sensitive, accurate, precise and reproducible UV spectrophotometric method for cefuroxime axetil using methanol as solvent. In this method the simple UV spectrum of cefuroxime axetil in methanol was obtained which exhibits absorption maxima (?max) at 278 nm. The quantitative determination of the drug was carried out at 278 nm and Beer’s law was obeyed in the range of (0.80-3.60) µg/ml. The proposed method was applied to pharmaceutical formulation and percent amount of drug estimated (95.6% and 96%) was found in good agreement with the label claim. The developed method was successfully validated with respect to linearity, specificity, accuracy and precision. The method was shown linear in the mentioned concentrations having line equation y = 0.05x + 0.048 with correlation coefficient of 0.995. The recovery values for cefuroxime axetil ranged from 99.85-100.05. The relative standard deviation of six replicates of assay was less than 2%. The percent relative standard deviations of inter-day precision ranged between 1.45-1.92% and intra-day precision of cefuroxime axetil was 0.96-1.51%. Hence, proposed method was precise, accurate and cost effective.  Keywords: UV-Vis spectrophotometer; Method validation; Cefuroxime axetil; Recovery studies.  © 2013 JSR Publications. ISSN: 2070-0237 (Print); 2070-0245 (Online). All rights reserved.   doi: http://dx.doi.org/10.3329/jsr.v6i1.14879 J. Sci. Res. 6 (1), 133-141 (2013)  

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