scholarly journals Validation and Optimization of a Simple RP-HPLC Method for Determination of Trimetazidine in Human Serum and its Application in a Pharmacokinetic Study with Healthy Bangladeshi Male Volunteers

2012 ◽  
Vol 10 (2) ◽  
pp. 71-78 ◽  
Author(s):  
Md Mazharul Islam Chowdhury ◽  
Md Ashik Ullah ◽  
Abdullah Al Maruf ◽  
Mohammad Safiqul Islam ◽  
Maizbha Uddin Ahmed ◽  
...  
Keyword(s):  
Human Serum ◽  
Pharmacokinetic Study ◽  
Potassium Dihydrogen Phosphate ◽  
Internal Standard ◽  
Hplc Method ◽  
Precipitation Method ◽  
Dihydrogen Phosphate ◽  
Serum Samples ◽  
Limit Of Quantification ◽  
Relative Standard

Trimetazidine is an effective and well-tolerated antianginal drug. In the present study, a simple, sensitive  and specific liquid chromatography (HPLC) method with UV detection was developed and validated for the  quantification of trimetazidine in human serum samples using caffeine as internal standard. Protein precipitation  method with methanol was employed in the extraction of trimetazidine and caffeine from biological matrix. The  chromatographic separation was accomplished on Xterra C18 Column with a mobile phase consisting 0.01 M  potassium dihydrogen phosphate buffer (pH 4.16 ± 0.01 adjusted with orthophosphoric acid, with a solvent system of  triethanolamine and acetonitrile (90:10) at a flow rate of 1.0 ml/min. The chromatogram was monitored at a  wavelength of 207 nm. The method was validated over a linear concentration range of 5-200 ng/ml and limit of  quantification (LOQ) was 5.0 ng/ml with a coefficient of correlation (r2) ? 0.996. The intra-day and inter-day  precision expressed as relative standard deviation was 3.40%-11.63% and 1.30%-10.21%, respectively. The average  recovery of trimetazidine from serum was 97.44%. The method was successfully applied to a pharmacokinetic study  after oral administration of modified release trimetazidine hydrochloride tablet (35 mg) in healthy Bangladeshi  volunteers. DOI: http://dx.doi.org/10.3329/dujps.v10i2.11783 Dhaka Univ. J. Pharm. Sci. 10(2): 71-78, 2011 (December)  

scholarly journals Validation and Optimization of a Simple RP-HPLC Method for the Determination of Paracetamol in Human Serum and its Application in a Pharmacokinetic Study with Healthy Bangladeshi Male Volunteers

2015 ◽  
Vol 13 (2) ◽  
pp. 125-131
Author(s):  
Anisa Alam Tanam ◽  
Mohammad Firoz Khan ◽  
Ridwan Bin Rashid ◽  
Md Zakir Sultan ◽  
Mohammad A Rashid
Keyword(s):  
Human Serum ◽  
Pharmacokinetic Study ◽  
Internal Standard ◽  
Immediate Release ◽  
Hplc Method ◽  
Serum Samples ◽  
Limit Of Quantification ◽  
Rp Hplc ◽  
Relative Standard

Acetaminophen (paracetamol) is an analgesic and antipyretic agent with minimum anti-inflammatory properties. In the present study a simple, fast, accurate, precise and reproducible RP-HPLC method has been developed and validated for the quantification of paracetamol in human serum samples using theophylline as internal standard. Protein precipitation with perchloric acid was employed in the extraction of paracetamol and theophylline from biological matrix. The chromatographic separation was accomplished on Phenomenex C18 column with a mobile phase comprising of 0.05 mM sodium sulfate buffer (pH 2.2 ± 0.02 adjusted with phosphoric acid) and acetonitrile at a ratio of 93:7 at a flow rate of 1.0 ml/min. The chromatogram was monitored by UV detection at a wavelength of 254 nm. The method was validated over a linear concentration range of 2-100 ?g/ml and limit of quantification (LOQ) was 1.61 ?g/ml with a correlation coefficient (r2) 0.997. The intra-day and inter-day precision expressed as relative standard deviation were found to be 0.49 - 2.68% and 0.36 - 3.44%, respectively. The average recovery of paracetamol from serum ranged from 99.0 - 106.4%. The method was successfully applied to a pharmacokinetic study after oral administration of immediate release paracetamol tablet (1000 mg) in four healthy Bangladeshi volunteers. The mean Cmax was found to be 11.03 ± 3.21 ?g/ml, which occurred at Tmax of 0.88 ± 0.14 hr. The half life, AUC0-8 and AUC0-? values were found to be 3.09 ± 0.71 hr, 31.06 ± 6.57 hr-?g/ml and 37.92 ± 9.51 hr- ?g/ml, respectively. DOI: http://dx.doi.org/10.3329/dujps.v13i2.21889 Dhaka Univ. J. Pharm. Sci. 13(2): 125-131, 2014 (December)

scholarly journals A Simple RP?HPLC Method for the Determination of Cefdinir in Human Serum: Validation and Application in a Pharmacokinetic Study with Healthy Bangladeshi Male Volunteers

2012 ◽  
Vol 10 (2) ◽  
pp. 109-116 ◽  
Author(s):  
Golam Mortuza Shahed ◽  
Md Ashik Ullah ◽  
Abdullah Al Abdullah Al ◽  
Maizbha Uddin Ahmed ◽  
Mohammad Safiqul Islam ◽  
...  
Keyword(s):  
Human Serum ◽  
Internal Standard ◽  
Hplc Method ◽  
Pharmacokinetic Parameters ◽  
Dihydrogen Phosphate ◽  
Serum Samples ◽  
Limit Of Quantification ◽  
Rp Hplc ◽  
Male Volunteers ◽  
The Mean

In the present study, a simple RP?HPLC method with UV detection has been validated to determine cefdinir concentrations in human serum samples and applied to determine the pharmacokinetic parameters of cefdinir in healthy Bangladeshi male volunteers. The mobile phase consisting of a mixture of 0.2 M sodium dihydrogen phosphate buffer (pH 3.2 ± 0.05 adjusted with o-phosphoric acid) and methanol at a ratio of 70:30 (v/v), was pumped at a flow rate of 1.0 ml/min through the C18 column at room temperature and the chromatographic separation was monitored at a wavelength of 254 nm with a sensitivity of 0.0001 AUFS. Cefaclor was used as internal standard. The developed method was selective and linear for cefdinir concentrations ranging from 0.05 to 5 ?g/ml for serum samples. The lower limit of quantification was defined as the lowest concentration on the calibration curve (0.05 ?g/ml) for which an acceptable accuracy of 111.60 % and a precision of 7.65 % were obtained, while the minimum detectable quantity of cefdinir was found to be 0.02 ?g/ml. The intra-day and inter-day coefficient of variation (CV) at 0.05 ?g/ml were 7.65% and 9.72%, respectively. The average recovery of cefdinir from serum was 96.43 %. Acceptable results were obtained during stability study. The mean Cmax of cefdinir was found to be 1.42 ± 0.53 ?g/ml attained at a mean Tmax of 3.81 ± 0.96 hr. The mean elimination half-life was 2.03 hours. This method proved to be simple, accurate and precise for pharmacokinetic and bioequivalence studies of cefdinir.   DOI: http://dx.doi.org/10.3329/dujps.v10i2.11790   Dhaka Univ. J. Pharm. Sci. 10(2): 109-116, 2011 (December)

scholarly journals Bioanalytical method validation of Esomeprazole by high performance liquid chromatography with PDA detection

2020 ◽  
Author(s):  
Fatema Moni ◽  
Suriya Sharmin ◽  
Satyajit Roy Rony ◽  
Farhana Afroz ◽  
Shammi Akhter ◽  
...  
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
High Performance ◽  
Limit Of Detection ◽  
Internal Standard ◽  
Precipitation Method ◽  
Dihydrogen Phosphate ◽  
Serum Samples ◽  
Bioanalytical Method Validation ◽  
Relative Standard

AbstractThis study describes the development and validation of a simple, specific, accurate, and precise method for quantitative determination of Esomeprazole in human serum using Pantoprazole as internal standard (IS). After the addition of internal standard, Esomeprazole from serum samples was extracted simply by protein precipitation method followed by centrifugation and the supernatants were directly injected into the high performance liquid chromatography (HPLC). The chromatographic separation of the compounds was obtained on Hitachi Lachrom C8 column (5 µm, 250 × 4.6 mm) with a mobile phase consisting of 5 mM potassium dihydrogen phosphate pH 7.4 and acetonitrile in a ratio of 70:30 with UV detection at 302 nm with a flow rate of 1 mL/min. The method was sensitive and specific, and validated over a concentration range of 0.06–6.0 µg/mL. The limit of detection (LOD) and lower limit of quantification (LOQ) was 0.03 µg/mL and 0.06 µg/mL, respectively. The precision and accuracy expressed as relative standard deviation were less than 15%. The average recovery of Esomeprazole from serum was 97.08%.

scholarly journals Validated RP-HPLC Method for the Assay of Etoricoxib (A Non-Steroidal Anti-Inflammatory Drug) in Pharmaceutical Dosage Forms

2012 ◽  
Vol 9 (2) ◽  
pp. 832-838 ◽  
Author(s):  
Srinivasu Topalli ◽  
T. G. Chandrashekhar ◽  
M. Mathrusri Annapurna
Keyword(s):  
High Performance ◽  
Limit Of Detection ◽  
Potassium Dihydrogen Phosphate ◽  
Internal Standard ◽  
High Performance Liquid Chromatographic ◽  
Dosage Forms ◽  
Hplc Method ◽  
Dihydrogen Phosphate ◽  
Limit Of Quantification ◽  
Pharmaceutical Dosage Forms

A simple, accurate, sensitive and reproducible reverse phase high performance liquid chromatographic method has been developed for the quantitative determination of Etoricoxib in pharmaceutical dosage forms. The assay was performed on Hypersil ODS C-18 (250 x 4.6 mm., 5µm particle size) column using acetonitrile and potassium dihydrogen phosphate buffer (pH 4.2) (46:54 % v/v) as mobile phase with UV detection at 280 nm (flow rate 1.2 ml/min). Bromhexine was used as an internal standard. Quantization was achieved by measurement of the peak area ratio of the drug to the internal standard. The limit of detection (LOD) and the limit of quantification (LOQ) were 0.0704 µg ml-1and 0.2134 µg ml-1respectively. Each analysis required no longer than 10 minutes. The calibration curve was linear over the concentration range from 0.5-85.0 µg ml-1. The retention times of Etoricoxib and Bromhexine were found to be 3.083 and 7.631 minutes respectively. The proposed method was validated according to the ICH guidelines and can be used successfully to analyse marketed formulations.

Simultaneous Determination of Chloroquine and Pyrimethamine with Cetirizine in an Active Form and Human Serum by RP-HPLC

2021 ◽  
Author(s):  
Hina Shamshad ◽  
Ali Sayqal ◽  
Jahan Zeb ◽  
Agha Zeeshan Mirza
Keyword(s):  
Human Serum ◽  
Simultaneous Determination ◽  
Active Form ◽  
Internal Standard ◽  
Hplc Method ◽  
Serum Samples ◽  
Rp Hplc ◽  
Cetirizine Hydrochloride ◽  
Bulk Drug

Abstract A simple, accurate and precise RP-HPLC method was developed for the simultaneous determination of chloroquine, pyrimethamine and cetirizine hydrochloride concentrations in bulk drug and human serum. The assay was performed using a mobile phase of methanol: water (70:30) at pH of 2.8 ± 0.05 on the Purospher C-18 column with UV detection at 230 nm and rosuvastatin used as an internal standard. The retention times observed for chloroquine, pyrimethamine and cetirizine hydrochloride were 3.5, 2.5 and 5.5 minutes, respectively. The method was found to be specific for the assayed drugs showing a linear response in the concentration range of 1–100 μg mL−1 with coefficients of determination values of (r = 0.999). The method was developed and validated according to ICH guidelines. The method was used to monitor the serum samples and was found to be sensitive for therapeutic purposes, showing the potential to be a useful tool for routine analysis in laboratories.

scholarly journals Quantitative Determination of Azithromycin in Human Plasma by Liquid Chromatography–Mass Spectrometry and its Application in Pharmackokinetic Study

2012 ◽  
Vol 11 (1) ◽  
pp. 55-63 ◽  
Author(s):  
Maizbha Uddin Ahmed ◽  
Mohammad Safiqul Islam ◽  
Tasmin Ara Sultana ◽  
AGM Mostofa ◽  
Muhammad Shahdaat Bin Sayeed ◽  
...  
Keyword(s):  
Mobile Phase ◽  
Solid Phase ◽  
Internal Standard ◽  
Extraction Process ◽  
Serum Samples ◽  
Limit Of Quantification ◽  
Relative Standard ◽  
Linear Concentration Range ◽  
Linear Concentration

Azithromycin is an effective and well-known antimicrobial agent. In the present study, a simple, sensitive and specific LC/MS/MS method has been developed and validated for the quantification of Azithromycin in  human serum samples using Clarithromycin as internal standard. Azithromycin was extracted from biological matrix  by using solid phase extraction process. The chromatographic separation was performed on Luna C18 (3 ?, 2x150   mm) column with a mobile phase consisting of 35 mM ammonium acetate buffer (mobile phase-A) and acetonitrile  and methanol in ratio of 90:10 ( as mobile phase-B) at a flow rate of 0.25 mL/min. The method was validated over a  linear concentration range of 0.5?50.0 ng/mL and limit of quantification (LOQ) was 0.5 ng/mL with a coefficient of  correlation (r2) = 0.9998. The intra-day and inter-day precision expressed as relative standard deviation were 1.64% – 8.43% and 2.32% – 9.92%, respectively. The average recovery of azithromycin from serum was 98.11%. The method  was successfully applied to a pharmacokinetic study after oral administration of Azithromycin 200 mg/5 ml suspension in healthy Bangladeshi volunteers. DOI: http://dx.doi.org/10.3329/dujps.v11i1.12488 Dhaka Univ. J. Pharm. Sci. 11(1): 55-63, 2012 (June)

scholarly journals HPLC-UV method for quantification of favipiravir in pharmaceutical formulations

2020 ◽  
Author(s):  
İbrahim Bulduk
Keyword(s):  
High Performance ◽  
Potassium Dihydrogen Phosphate ◽  
Pharmaceutical Formulations ◽  
Hplc Method ◽  
Dihydrogen Phosphate ◽  
Potential Candidate ◽  
Column Temperature ◽  
Candidate Drug ◽  
System Suitability ◽  
Relative Standard

AbstractFavipiravir (FVP), a pyrazine analog, has shown antiviral activity against a wide variety of viruses. It is considered to be worth further investigation as a potential candidate drug for COVID-19. It is not officially available in any pharmacopoeia. A rapid, simple, precise, accurate, and isocratic high performance liquid chromatography (HPLC) method has been developed for routine quality control of favipiravir in pharmaceutical formulations. Separation was carried out by C18 column. The mobile phase was a mixture of 50 mM potassium dihydrogen phosphate (pH 2.3) and acetonitrile (90:10, v/v) at a flow rate of 1 mL min−1. The ultraviolet (UV) detection and column temperature were 323 nm, and 30 °C, respectively. The run time was 15 min under these chromatographic conditions. Excellent linear relationship between peak area and favipiravir concentration in the range of 10–100 μg mL−1 has been observed (r2, 0.9999). Developed method has been found to be sensitive (limits of detection and quantification were 1.20 μg mL−1 and 3.60 μg mL−1, respectively), precise (the interday and intraday relative standard deviation (RSD) values for peak area and retention time were less than 0.4 and 0.2%, respectively), accurate (recovery, 99.19–100.17%), specific and robust (% RSD were less than 1.00, for system suitability parameters). Proposed method has been successfully applied for quantification of favipiravir in pharmaceutical formulations.

scholarly journals Validation of developed method by RP-HPLC for estimation of Prasugrelin human plasma and studying the stability of the drugs in plasma

2018 ◽  
Vol 13 (1) ◽  
pp. 65-75
Author(s):  
Kumar S. Ashutosh ◽  
Debnath Manidipa ◽  
Rao J.V.L.N. Seshagiri ◽  
Sankar D. Gowri
Keyword(s):  
Human Plasma ◽  
High Performance ◽  
Method Development ◽  
Potassium Dihydrogen Phosphate ◽  
Array Detector ◽  
Dihydrogen Phosphate ◽  
Limit Of Quantification ◽  
Rp Hplc ◽  
Relative Standard ◽  
The Stability

This paper is concern with a reverse phase high performance liquid chromatography (RP-HPLC) bio-analytical method development and validation for Prasugrel in human plasma using photo diode array detector (PDA detector). The HPLC separation was carried out in an isocratic mode on an X-Terra C18 column (4.6 x 150 mm; 5 μm) with a mobile phase consisting of potassium dihydrogen phosphate [pH 3.0] and acetonitrile in the ratio of 30:70 v/v at a flow rate of 1.0 mL/min. The run time was maintained for 5 mins and the detection was monitored at 210 nm. The percentage recovery was found 99.61-100.06 in human plasma. This reveals that the method is quite accurate. The linearity was found 15-40 μg/mL in human plasma. The inter-day and intra-day precision in plasma was found within the limits. The lower limit of quantification (LLOQ) obtained by the proposed method was 0.05 μg/mL. The percentage relative standard deviation (%RSD) obtained for the drug spiked in plasma for stability studies were less than 2 %.Kathmandu University Journal of Science, Engineering and TechnologyVol. 13, No. 1, 2017, Page: 65-75

scholarly journals A Simple RP-HPLC Method for the Determination of Omeprazole in Human Serum and Urine: Validation and Application in Pharmacokinetic Study

1970 ◽  
Vol 8 (2) ◽  
pp. 123-130 ◽  
Author(s):  
Kamrun Nahar ◽  
Jafreen Jamal Joti ◽  
Md Ashik Ullah ◽  
Ahasanul Hasan ◽  
Mohammad Abul Kalam Azad ◽  
...  
Keyword(s):  
Human Serum ◽  
Hplc Method ◽  
Stability Study ◽  
Urine Samples ◽  
Dihydrogen Phosphate ◽  
Serum Samples ◽  
Rp Hplc ◽  
Limit Of Quantitation ◽  
Serum And Urine ◽  
Serum And Urine Samples

A Simple RP-HPLC method with UV detection has been validated to determine omeprazole concentrations in human serum and urine samples. The mobile phase consisted of a mixture of potassium dihydrogen phosphate buffer (pH 7.2 ± 0.05; 0.2 M) and acetonitrile (70:30, v/v), pumped at a flow rate of 1.0 ml/min through the C-8 column at room temperature. Peaks were monitored by UV absorbance at 302 nm at a sensitivity of 0.0001. The developed method was selective and linear for omeprazole concentrations ranging between 5 to 1000ng/ml for serum samples and 1 to 100μg/ml for urine samples. The recovery of omeprazole ranged from 95.68 to 99% and 95.54 to 99.8% for the serum and urine samples respectively. The limit of quantitation (LOQ) of omeprazole was 5 ng/ml. The intraday accuracy ranged from 93.54 to 104.38% and 100.55 to 103.48% for the serum and urine respectively. The interday accuracy varied from 97.61 to 113.95% and 97.42 to 109.97% for the serum and urine respectively. For the LOQ, good values of precision (6.03 and 10.13% for intraday and interday, respectively) were also obtained. Acceptable results were obtained during stability study. This method proved to be simple, accurate and precise for pharmacokinetic and bioequivalence studies of omeprazole. Key words: Omeprazole; RP-HPLC; Method validation. DOI: 10.3329/dujps.v8i2.6026 Dhaka Univ. J. Pharm. Sci. 8(2): 123-130, 2009 (December)

scholarly journals A Novel and Rapid RP-HPLC Quantitative Method for the estimation of Canagliflozin in Human Plasma

2021 ◽  
Vol 12 (1) ◽  
pp. 93-101
Author(s):  
Ajitha A ◽  
Sujatha K ◽  
Abbulu K
Keyword(s):  
Human Plasma ◽  
High Performance ◽  
Quantitative Estimation ◽  
Wave Length ◽  
Potassium Dihydrogen Phosphate ◽  
Internal Standard ◽  
Accurate Method ◽  
Dihydrogen Phosphate ◽  
Chromatographic Technique ◽  
Limit Of Quantification

A simple, precise and accurate method was developed for the quantitative estimation of Canagliflozin in human plasma using Dapagliflozin as internal standard by Reverse Phase-High Performance Liquid Chromatographic technique. Chromatographic conditions were of stationary phase Phenomenex Luna C18 (2) (150 x 4.6 mm, 5m), Mobile phase 0.01 N Potassium dihydrogen Phosphate buffer pH (3.5±0.05) : acetonitrile in the ratio of 45:55 and flow rate at 1.0 ml/min, detection wave length was UV 222 nm, column oven temperature was maintained at 30ᵒC, and sample injection volume of 10 µL. Retention time of Canagliflozin was found to be about 8.7 min. Coefficient of Variation for Canagliflozin peak was 3.15 %, % recovery was 94.58 %. The linearity of method was studied from 0.06 µg/ml to 2.4 µg/ml (R2 = 0.999). The Signal to Noise ratio of lower limit of quantification (0.06 µg/ml) was found to be 50. The proposed bio-analytical method was validated by following ICH guidelines.

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