The Dtermination of Paracetamol by HPLC Validation of the Method and Application on Serum Samples

2018 ◽  
Vol 69 (3) ◽  
pp. 627-631 ◽  
Author(s):  
Viorica Ohriac (Popa) ◽  
Diana Cimpoesu ◽  
Adrian Florin Spac ◽  
Paul Nedelea ◽  
Voichita Lazureanu ◽  
...  

Pain is defined as a disagreeable sensory and emotional experience related to a tissue or potential lesion. Paracetamol (Acetaminophen) is the most used non-morphine analgesic. For the determination of paracetamol we developed and validated the high performance liquid chromatography (HPLC) analysis using a Dionex Ultimate 3000 liquid chromatograph equipped with a multidimensional detector. After determining the optimum conditions of analysis (80/20 water / acetonitrile mobile phase, flow rate 1.0 mL / min, detection wavelength 245 nm) we validated the method following the following parameters: linearity of response function, linearity of results, limit (LD = 0.66 mg / mL) and quantification limit (LQ = 2.00 mg / mL), and precision. The method of determining paracetamol by HPLC was applied to 30 samples of serum collected from patients who had pain and were treated with paracetamol.

1994 ◽  
Vol 59 (3) ◽  
pp. 569-574 ◽  
Author(s):  
Josef Královský ◽  
Marta Kalhousová ◽  
Petr Šlosar

The reversed-phase high-performance liquid chromatography of some selected, industrially important aromatic sulfones has been investigated. The chromatographic behaviour of three groups of aromatic sulfones has been studied. The optimum conditions of separation and UV spectra of the sulfones and some of their hydroxy and benzyloxy derivatives are presented. The dependences of capacity factors vs methanol content in mobile phase are mentioned. The results obtained have been applied to the quantitative analysis of different technical-grade samples and isomer mixtures. For all the separation methods mentioned the concentration ranges of linear calibration curves have been determined.


1985 ◽  
Vol 4 (3) ◽  
pp. 317-322 ◽  
Author(s):  
F. Plavsic ◽  
J. Čulig

Diclofenac was isolated from plasma by double extraction with organic solvent. Chromatography was performed on Lichrosorb NH2 column with acetonitrile and perchloric acid (0.0025 mol/l; 35:65, v/v) as the mobile phase (flow rate 0.9 ml/min). The electrochemical detector was operated at +900 mV and sensitivity of 5-10 nA. The sensitivity of the method was 10 μg/1 and the coefficients of variation below 10% in the entire range of the concentration in a dose interval.


2020 ◽  
Vol 11 (3) ◽  
pp. 3846-3849
Author(s):  
Ashok P ◽  
Narenderan S T ◽  
Meyyanathan S N ◽  
Babu B ◽  
Jawahar N

The present study was aimed to develop and validate a simple, sensitive and economical bio-analytical high-performance liquid chromatographicultraviolet method for the determination of irbesartan in human plasma. The method involves the use of simple precipitation method for the determination of irbesartan, using methanol as precipitating agent and losartan as internal standard. The separation was achieved using Zorbax C18 column (150 x 4.6 mm, 5µm), mobile phase consists of methanol and 0.2% formic acid in water at the ratio 85:15, v/v using detection wavelength of 237 nm. Further, the developed method was validated as per US-FDA guidelines for accuracy, precision, linearity, stability, detection and quantification limit. The method developed was found to be linear over the concentration ranging from 5 to 500 ng/ml with a correlation coefficient of 0.9987. The LOD and LLOQ of the method were found to be 1 ng/ml and 5 ng/ml, respectively.


2018 ◽  
Vol 69 (2) ◽  
pp. 297-299
Author(s):  
Adriana Nita ◽  
Delia Mirela Tit ◽  
Lucian Copolovici ◽  
Carmen Elena Melinte (Frunzulica) ◽  
Dana Maria Copolovici ◽  
...  

The aim of this study was to develop and validate a rapid, accurate, and exact method for the quantitative determination of famotidine in pharmaceutical products. The HPLC analyses were performed by using a mobile phase containing methanol:1% acetic acid solution=30:7 (v/v), at a flow rate of 0.4 mL/min.The total time of the method was 10 min, and the retention time of famotidine was 4.16 min. The detection was evaluated at l=267 nm. The method has been validated by using different validation parameters. The linear response of the detector for famotidine peak area was observed at concentrations ranging from 0.1 to 0.0001 mg mL-1 , resulting in a correlation coefficient of 0.99998. The values of the detection limit and of the quantification limit are 0.00048 mg mL-1 and 0.00148 mg mL-1, respectively. The method proposed allowed accurate (with a relative error of less than 2%) and precise (RSD values less than 2.0%) determination of famotidine content in pharmaceutical products and can be used for its rapid quantitative analysis.


2018 ◽  
Vol 15 (1) ◽  
pp. 32-38 ◽  
Author(s):  
Bürge Aşçı ◽  
Mesut Koç

Introduction:This paper presents the development and validation of a novel, fast, sensitive and accurate high performance liquid chromatography (HPLC) method for the simultaneous quantitative determination of dibucaine HCl, fluocortolone pivalate and fluocortolone caproate in pharmaceutical preparations.Experiment:Development of the chromatographic method was based on an experimental design approach. A five-level-three-factor central composite design requiring 20 experiments in this optimization study was performed in order to evaluate the effects of three independent variances including mobile phase ratio, flow rate and amount of acid in the mobile phase.Conclusion:The optimum composition for mobile phase was found as a methanol:water:acetic acid mixture at 71.6 : 26.4 : 2 (v/v/v) ratio and optimum separation was acquired by isocratic elution with a flow rate of 1.3 mL/min. The analytes were detected using a UV detector at 240 nm. The developed method was validated in terms of linearity, precision, accuracy, limit of detection/quantitation and solution stability and successfully applied to the determination of dibucaine HCl, fluocortolone pivalate and fluocortolone caproate in pharmaceutical topical formulations such as suppositories and ointments.


Amino Acids ◽  
2021 ◽  
Author(s):  
Grażyna Gałęzowska ◽  
Joanna Ratajczyk ◽  
Lidia Wolska

AbstractThe quantitation and qualification of amino acids are most commonly used in clinical and epidemiological studies, and provide an excellent way of monitoring compounds in human fluids which have not been monitored previously, to prevent some diseases. Because of this, it is not surprising that scientific interest in evaluating these compounds has resurfaced in recent years and has precipitated the development of a multitude of new analytical techniques. This review considers recent developments in HPLC analytics on the basis of publications from the last few years. It helps to update and systematize knowledge in this area. Particular attention is paid to the progress of analytical methods, pointing out the advantages and drawbacks of the various techniques used for the preparation, separation and determination of amino acids. Depending on the type of sample, the preparation conditions for HPLC analysis change. For this reason, the review has focused on three types of samples, namely urine, blood and cerebrospinal fluid. Despite time-consuming sample preparation before HPLC analysis, an additional derivatization technique should be used, depending on the detection technique used. There are proposals for columns that are specially modified for amino acid separation without derivatization, but the limit of detection of the substance is less beneficial. In view of the fact that amino acid analyses have been performed for years and new solutions may generate increased costs, it may turn out that older proposals are much more advantageous.


2006 ◽  
Vol 830 (2) ◽  
pp. 231-237 ◽  
Author(s):  
Lata Kaphalia ◽  
Bhupendra S. Kaphalia ◽  
Santosh Kumar ◽  
Mary F. Kanz ◽  
Mary Treinen-Moslen

2011 ◽  
Vol 8 (1) ◽  
pp. 340-346 ◽  
Author(s):  
Rajesh M. Kashid ◽  
Santosh G. Singh ◽  
Shrawan Singh

A reversed phase HPLC method that allows the separation and simultaneous determination of the preservatives methyl paraben (M.P.) and propyl paraben (P.P.) is described. The separations were effected by using an initial mobile phase of water: acetonitrile (50:50) on Inertsil C18 to elute P.P. and M.P. The detector wavelength was set at 205 nm. Under these conditions, separation of the two components was achieved in less than 10 min. Analytical characteristics of the separation such as precision, specificity, linear range and reproducibility were evaluated. The developed method was applied for the determination of preservative M.P. and P.P. at concentration of 0.01 mg/mL and 0.1 mg/mL respectively. The method was successfully used for determining both compounds in sucralfate suspension.


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