Quantification of Pyrazinamide in Human Plasma by Validated High Performance Liquid Chromatography Method

2021 ◽  
Vol 15 (10) ◽  
pp. 2896-2899
Author(s):  
Waleed Arshad ◽  
Naseem Saud Ahmad ◽  
Abdul Muqeet Khan ◽  
Iram Imran ◽  
Qura- Tul-Ain ◽  
...  

Objective: To be able to accurately determine the quantity of Pyrazinamide (PZA) in different tablet preparations and human plasma using an Ultra violet detector equipped high performance liquid chromatography (HPLC). Study Design: Experimental study Place and Duration of Study: Department of Bioequivalence Studies, University of Veterinary and Animal Sciences Lahore and the Department of Pharmacology, University of Health Sciences, Lahore the from 1st April 2017 to 31st March 2018. Methodology: Two mobile phases were used, the first compromised of disodium hydrogen phosphate buffer having a pH of 6.8 and acetonitrile in the proportion of (95:5) and the second was a combination of aforesaid substances in equivalent proportion (50:50 v/v). The gradient for the first 5 min was exclusively Mobile phase “a” after which 5-6 min Mobile phase “b” was raised from 0 to 100% and was kept at 100% till the completion of the cycle. The flow of mobile phase was kept at 1000 µl/min. Determination of PZA was done using a ultraviolet detector at a wavelength of 238 nm. Amount of sample injected was 40 μl. Procedure was done by using Shizmadu Chromatographic System, Japan equipped with a SIL-20AC HT auto-sampler, SPD-M20A, CTO 20 AC, a LC-20AT VP pump, and CBM 20A controller unit. A C18 column was used as well. Results: Retention time of PZA was 6.1±2%. Precision was 0.46 to 2.20% relative standard deviation for intra assay and for inter assay we obtained 0.29 to 34.45% RSD for all quality control levels. The overall recovery of PZA was 96.75%. Conclusion: High selectivity for PZA was seen and no other spikes from drugs present in FDC regimen were observed at the time when PZA is detected in blank plasma samples Key words: Chromatography, High pressure liquid. Pyrazinamide. Tuberculosis

2017 ◽  
Vol 2017 ◽  
pp. 1-7
Author(s):  
Paula Karina S. Uchoa ◽  
Leandro Bezerra de Lima ◽  
Antonia T. A. Pimenta ◽  
Maria da Conceição F. de Oliveira ◽  
Jair Mafezoli ◽  
...  

A high-performance liquid chromatography method was developed and validated for the quantification of the cytotoxic compounds produced by a marine strain ofAspergillus niger. The fungus was grown in malt peptone dextrose (MPD), potato dextrose yeast (PDY), and mannitol peptone yeast (MnPY) media during 7, 14, 21, and 28 days, and the natural products were identified by standard compounds. The validation parameters obtained were selectivity, linearity (coefficient of correlation > 0.99), precision (relative standard deviation below 5%), and accuracy (recovery > 96).


INDIAN DRUGS ◽  
2013 ◽  
Vol 50 (07) ◽  
pp. 14-21
Author(s):  
S. Sahu ◽  
◽  
R.M Singh ◽  
S.C. Mathur ◽  
D. K Sharma ◽  
...  

A simple, fast, precise and accurate ultra high performance liquid chromatography method was developed for degradation study of eletriptan hydrobromide (EH) under exaggerated conditions. An Inertsil ODS C18 (250 x 4.6 mm, 5µm) column in isocratic mode was used with mobile phase comprising of water, methanol and trifluoroacetic acid mixed in the ratio 55:45:0.1 % V/V/V, maintained at pH 3.5. The flow rate was set at 0.4 mL per minute with UV detection at 225 nm. The retention time of EH was found to be 3.7 minutes. Linearity for EH was found in the range of 3.5- 200 µg per mL and percentage recoveries were obtained in the range of 100.2 % to 100.6 %. The method was capable of resolving all degradants and principle component in sample. The proposed method is accurate, precise, selective, reproducible, and rapid for detection of degradation of eletriptan hydrobromide.


Author(s):  
Mannem Durga Babu ◽  
Kesana Surendrababu

Objective: The objective of the study was to develop and validate a novel, specific, precise, and simple reversed-phase high-performance liquid chromatography method for the estimation of guaifenesin present in methocarbamol API and its pharmaceutical dosage forms. Methods: The baseline separation for methocarbamol and guaifenesin was achieved by utilizing a Inertsil ODS C18 (250 mm × 4.6 mm) 5 μm column particle size and an isocratic elution method. The mobile phase contains a mixture of water and acetonitrile in the ratio of 70:30 v/v, respectively. The flow rate of the mobile phase was 1.0 mL/min with a column temperature of 25°C and detection wavelength at 272 nm. The method was validated for a limit of detection (LOD), limit of quantification (LOQ), linearity, accuracy, and reproducibility with the help of the exhibit and simulated samples. Results: The LOD for guaifenesin was 0.62 μg/mL. The LOQ for guaifenesin was 1.87 μg/mL. The correlation coefficient obtained for impurity was >0.99. The recovery was obtained for impurity was 106.56% at 50%, 95.20% at 100%, and 100.45% at 150%. In tablet analysis, we can found 0.26% (<0.5%). Conclusion: The developed method was validated as per the ICH guidelines with respect to specificity, precision, linearity, accuracy, LOD and quantification, ruggedness, robustness, and solution stability.


Author(s):  
K. SRI GIRIJA ◽  
BIKSHAL BABU KASIMALA ◽  
VENKATESWARA RAO ANNA

Objective: The objective of the present study is to develop a stability-indicating reverse-phase high-performance liquid chromatography (RP-HPLC) method for qualitative and quantitative determination of Eptifibatide and its impurities in bulk and pharmaceutical dosage forms. Methods: The chromatographic separation was carried on Phenomenex Luna C18 column (250 mm×4.6 mm; 5µ id) as stationary phase, methanol and phosphate buffer at pH 6.4 in the ratio of 65:45 (v/v) as mobile phase at flow rate of 1.0 ml/min, Ultra Violet (UV) detection was carried at the wavelength of 236 nm and the analysis was completed with a run time of 15 min. Results: In the developed conditions, the retention time of Eptifibatide and its impurities 1 and 2 were found to be 3.35, 4.93 and 8.18 min, respectively. The method was validated for system suitability, range of analysis, precision, specificity, stability and robustness. Spiked recovery at 50%, 100% and 150% was carried for both standard and impurities and the acceptable % recovery of 98-102 was observed for Eptifibatide and both impurities studied and the % Relative standard deviation (RSD) in each spiked level was found to be less than 2. Stability tests were done through the exposure of the analyte solution to five different stress conditions i. e expose to 1N Hydrochloric acid (HCl), 1 N Sodium hydroxide (NaOH), 3% Hydrogen peroxide (H2O2), 80 °C temperature to UV radiation. In all the degradation conditions, standard drug Eptifibatide was detected along with both the impurities studied and the degradation products were successfully separated. In the formulation analysis, there is no other chromatographic detection of other impurities and formulation excipients. Conclusion: The developed method was found to be suitable for the quantification of Eptifibatide and can separate and analyse impurities 1 and 2.


Chemija ◽  
2018 ◽  
Vol 29 (2) ◽  
Author(s):  
Audrius Markevičius ◽  
Audrius Zolumskis ◽  
Audrius Sadaunykas ◽  
Birutė Knašienė ◽  
Adrian Vicent Claramunt ◽  
...  

A fast, precise and accurate high performance liquid chromatography method has been developed for the determination of dyes (Solvent Red 19 and Solvent Blue 35) and a marker (Solvent Yellow 124) in diesel. Separation was carried out on a 250 × 4.60 mm Agilent Zorbax Rx-SIL column (5 µm particle size). Detection was done in a visible wavelength range. The best performance of fuel dye separation and the shortest retention times were achieved when using hexane, toluene and ethyl acetate as a mobile phase. During this research the eluent composition and the elution gradient were optimized consequently that helped to perform the analysis within 15 min. The developed method was applied for the analysis of real samples of dyed diesel fuel. Preparation of the samples for the analysis simply consisted of filtering through a 0.45 µm filter previous to direct injection of the sample into the HPLC system for analysis.


2010 ◽  
Vol 54 (8) ◽  
pp. 3408-3413 ◽  
Author(s):  
Lorena Baietto ◽  
Antonio D'Avolio ◽  
Giusi Ventimiglia ◽  
Francesco Giuseppe De Rosa ◽  
Marco Siccardi ◽  
...  

ABSTRACT We have developed and validated a high-performance liquid chromatography method coupled with a mass detector to quantify itraconazole, voriconazole, and posaconazole using quinoxaline as the internal standard. The method involves protein precipitation with acetonitrile. Mean accuracy (percent deviation from the true value) and precision (relative standard deviation percentage) were less than 15%. Mean recovery was more than 80% for all drugs quantified. The lower limit of quantification was 0.031 μg/ml for itraconazole and posaconazole and 0.039 μg/ml for voriconazole. The calibration range tested was from 0.031 to 8 μg/ml for itraconazole and posaconazole and from 0.039 to 10 μg/ml for voriconazole.


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