scholarly journals Improved HPLC Method for Determination of Four PPIs, Omeprazole, Pantoprazole, Lansoprazole and Rabeprazole in Human Plasma

2010 ◽  
Vol 13 (1) ◽  
pp. 1 ◽  
Author(s):  
Maryam Noubarani ◽  
Fariborz Keyhanfar ◽  
Manijeh Motevalian ◽  
Masoud Mahmoudian
Keyword(s):  
Human Plasma ◽  
Room Temperature ◽  
Internal Standard ◽  
Cost Benefit ◽  
Hplc Method ◽  
Single Step ◽  
Pharmacokinetic Studies ◽  
Limit Of Quantification ◽  
Liquid Liquid Extraction

ABSTRACT-PURPOSE: To develop a simple and rapid HPLC method for measuring of four proton-pump inhibitors (PPIs), omeprazole (OPZ), pantoprazole (PPZ), lansoprazole (LPZ) and rabeprazole (RPZ) concentrations in human plasma. METHODS: Following a single step liquid–liquid extraction analytes along with an internal standard (IS) were separated using an isocratic mobile phase of phosphate buffer (10 mM)/acetonitrile (53/47, v/v adjusted pH to 7.3 with triethylamine) at flow rate of 1 mL/min on reverse phase TRACER EXCEL 120 ODS-A column at room temperature. RESULTS: Total analytical run time for selected PPIs was 10 min. The assays exhibited good linearity (r2>0.99) over the studied range of 20 to 2500 ng/mL for OPZ, 20 to 4000 ng/mL for PPZ, 20 to 3000 ng/mL for LPZ and 20 to 1500 ng/mL for RPZ. The recovery of method was equal or greater than 80% and lower limit of quantification (LLOQ) was 20 ng/mL for four PPIs. Coefficient of variation and error at all of the intra-day and inter-day assessment were less than 9.2% for all compounds. CONCLUSIONS: The results indicated that this method is a simple, rapid, precise and accurate assay for determination of four PPIs concentrations in human plasma. This validated method is sensitive and reproducible enough to be used in pharmacokinetic studies and also is time- and cost-benefit when selected PPIs are desired to be analyzed.

scholarly journals Improved HPLC Method for the Determination of Moxifloxacin in Application to a Pharmacokinetics Study in Patients with Infectious Diseases

2013 ◽  
Vol 2013 ◽  
pp. 1-7 ◽  
Author(s):  
Nan Wang ◽  
Liqin Zhu ◽  
Xuequn Zhao ◽  
Wenjie Yang ◽  
He Sun
Keyword(s):  
Human Plasma ◽  
High Performance ◽  
Room Temperature ◽  
Internal Standard ◽  
Hplc Method ◽  
Single Step ◽  
Pharmacokinetic Studies ◽  
Liquid Liquid Extraction ◽  
High Concentrations

Objective. To develop a simple and rapid high-performance liquid chromatography (HPLC) method for measuring moxifloxacin concentration in human plasma. Methods. Following a single step liquid-liquid extraction, analytes along with an internal standard (IS) were separated using an isocratic mobile phase of 0.1% triethylamine (adjusted pH to 4.8 with phosphoric acid)/acetonitrile (80/20, v/v) at flow rate of 1 mL/min on reverse phase Kromasil C18 column (250 mm × 4.6 mm, 5 μm) at room temperature. Results. Total analytical run time for selecting moxifloxacin was 15 min. The assays exhibited good linearity (r2=0.9998) over the studied range of 25 to 5000 ng/mL. The absolute recovery rate of low, medium, and high concentrations were 69.88%, 78.86%, and 78.51%, respectively. The relative recovery rates were 98.50%, 96.61%, and 101.79%, respectively. Coefficient of variation and error at both of the intraday and interday assessments were less than 4.7%. Conclusions. The results indicated that this method is a simple, rapid, precise and accurate assay for the determination of moxifloxacin concentrations in human plasma. This validated method is sensitive and reproducible enough to be used in pharmacokinetic studies.

scholarly journals Determination of nimodipine in plasma by HPLC-MS/MS and pharmacokinetic application

2010 ◽  
Vol 46 (4) ◽  
pp. 665-677 ◽  
Author(s):  
Demétrius Fernandes do Nascimento ◽  
Manoel Odorico de Moraes ◽  
Fernando Antônio Frota Bezerra ◽  
Andréa Vieira Pontes ◽  
Célia Regina Amaral Uchoa ◽  
...  
Keyword(s):  
Human Plasma ◽  
Internal Standard ◽  
Pharmacokinetic Profile ◽  
Plasma Samples ◽  
Linear Calibration ◽  
Limit Of Quantification ◽  
Standard Curve ◽  
Liquid Liquid Extraction ◽  
Highly Sensitive

To develop and validate a rapid, specific and highly sensitive method to quantify nimodipine in human plasma using dibucaine as the internal standard (IS). The analyte and IS were extracted from plasma samples by liquid-liquid extraction using hexane-ethyl acetate (1:1 v/v). The chromatographic separation was performed on a Varian® Polaris C18 analytical column (3 μm, 50 x 2.0 mm) and pre-column SecurityguardTM C18 (4.0 x 3.0 mm) with a mobile phase of Acetonitrile-Ammonium acetate 0.02 ml/L (80:20v/v). The method had a chromatographic run time of 4.5 min and linear calibration curve over the range of 0.1- 40 ng/mL (r > 0.9938). The limit of quantification was 100 pg/mL. Acceptable precision and accuracy were obtained for concentrations over the standard curve ranges. This validated method was successfully applied in determining the pharmacokinetic profile of nimodipine tablets of 30 mg administered to 24 healthy volunteers. The proposed method of analysis provided a sensitive and specific assay for nimodipine determination in human plasma. The time for the determination of one plasma sample was 4.5 min. This method is suitable for the analysis of nimodipine in human plasma samples collected for pharmacokinetic, bioavailability or bioequivalence studies in humans.

scholarly journals A New Validated RP- HPLC Method for the Determination of Nevirapine in Human Plasma

2010 ◽  
Vol 7 (3) ◽  
pp. 821-826 ◽  
Author(s):  
C. H. Venkata Kumar ◽  
D. Ananth Kumar ◽  
J. V. L. N. Seshagiri Rao
Keyword(s):  
Human Plasma ◽  
High Performance ◽  
Ammonium Acetate ◽  
Internal Standard ◽  
High Performance Liquid Chromatographic ◽  
Hplc Method ◽  
Pharmacokinetic Studies ◽  
Liquid Chromatographic Method ◽  
Liquid Chromatographic

A rapid, selective and sensitive high performance liquid chromatographic method for the estimation of nevirapine in human plasma has been developed. Chromatography was carried out on a Hypersil BDS C18column using a mixture of ammonium acetate buffer (pH 4.0 ± 0.05) and acetonitrile (85:15 v/v) as the mobile phase. The eluents were monitored for the drug by UV detection at 254 nm. Oxcarbazepine was used as an internal standard for this study. The retention times for nevirapine and oxcarbazepine were found to be 7.2 and 14.7 min respectively. The method was found to be linear in the concentration range of 50 ng/mL to 5003.7 ng/mL. The method was validated as per FDA guidelines and was found to be suitable for bioequivalence and pharmacokinetic studies.

scholarly journals Development and Validation of Novel HPLC Bioanalytical Analysis Method for Acalabrutinib: An Anticancer Drug in Human Plasma

2020 ◽  
Vol 32 (10) ◽  
pp. 2606-2610
Author(s):  
G. Atchutarama Krishna ◽  
P. Srinivasarao ◽  
T. Benarji Patrudu ◽  
R. Chidanandaswamy
Keyword(s):  
Human Plasma ◽  
Orthophosphoric Acid ◽  
Internal Standard ◽  
Hplc Method ◽  
Linear Calibration ◽  
Liquid Liquid Extraction ◽  
Ich Guidelines ◽  
Relative Standard ◽  
Development And Validation

The aim of the work is to develop and validate the bioanalytical RP-HPLC method for determination of acalabrutinib in plasma with nifedipine drug as internal standard. Liquid-liquid extraction with diethyl ether and methanol in the ratio of 50:50 (v/v) was used for the extraction of drugs from the biological matrix. The optimized chromatography conditions consist of methanol, acetonitrile and 0.1% orthophosphoric acid in the ratio of 45:35:20 (v/v) as a mobile phase with KNAUER Eurospher II C18 Column (250 × 4.6 mm, 5μ) as stationary phase. Isocratic elution with 0.9 mL flow separates acalabrutinib at 4.6 min and nifedipine at 6.8 min. The method was validated as per ICH guidelines and linear calibration curve was obtained for the peak area ratio of acalabrutinib and nifedipine compound across a range of 50-3000 ng/mL. Greater than 90% recoveries were obtained for acalabrutinib. The relative standard deviation (%RSD) was found to be < 5% for precision studies. Hence, the method was found to be suitable for the analysis of acalabrutinib in spiked human plasma and is used for the pharmacokinetic study

scholarly journals LC-MS-MS Method for Determination of Metolazone in Human Plasma

2008 ◽  
Vol 5 (3) ◽  
pp. 634-640 ◽  
Author(s):  
Shikha M. N. Roy ◽  
Kiran V. Mangaonkar ◽  
Santosh. M. Yetal ◽  
Santosh. S. Joshi
Keyword(s):  
Human Plasma ◽  
High Performance ◽  
Extraction Procedure ◽  
Internal Standard ◽  
Bioequivalence Study ◽  
Specific Method ◽  
Simple Liquid ◽  
Limit Of Quantification ◽  
Liquid Liquid Extraction

A rapid, sensitive and specific method for quantification of metolazone in human plasma using metaxalone as internal standard is described. Sample preparation involved a simple liquid-liquid extraction procedure. The extract was analyzed by high performance liquid chromatography coupled to electrospray tandem mass spectrometry (LC–MS–MS). Chromatography was performed isocratically on a 5 μm C18analytical column (50 mm × 4.6 mmi.d.) with buffer–acetonitrile 20:80 (v/v) as mobile phase. The response to metolazone was a linear function of concentration over the range 1.00 to 2000.00 ng mL-1. The lower limit of quantification in plasma was 1.0 ng mL-1. The method was successfully applied in a bioequivalence study of a metolazone formulation after administration as a single oral dose.

Development and Validation of a New Method for the Determination of Anti-hepatitis C Agent Simeprevir in Human Plasma using HPLC with Fluorescence Detection

2020 ◽  
Vol 16 (4) ◽  
pp. 428-435
Author(s):  
Ahmed F.A. Youssef ◽  
Yousry M. Issa ◽  
Kareem M. Nabil
Keyword(s):  
Hepatitis C ◽  
Human Plasma ◽  
Fluorescence Detection ◽  
Internal Standard ◽  
Protein Precipitation ◽  
Assay Method ◽  
Fluorescence Detector ◽  
Limit Of Quantification ◽  
Relative Standard

Background: Simeprevir is one of the recently discovered drugs for treating hepatitis C which is one of the major diseases across the globe. Objective: The present study involves the development of a new and unique High-Performance Liquid Chromatography (HPLC) method using fluorescence detection for the determination of simeprevir (SIM) in human plasma. Methods: Two methods of extractions were tested, protein precipitation using acetonitrile and liquidliquid extraction. A 25 mM dipotassium hydrogen orthophosphate (pH 7.0)/ACN (50/50; v/v), was used as mobile phase and C18 reversed phase column as the stationary phase. The chromatographic conditions were optimized and the concentration of simeprevir was determined by using the fluorescence detector. Cyclobenzaprine was used as an internal standard. Results: Recovery of the assay method based on protein precipitation was up to 100%. Intra-day and inter-day accuracies range from 92.30 to 107.80%, with Relative Standard Deviation (RSD) range 1.65-8.02%. The present method was successfully applied to a pharmacokinetic study where SIM was administered as a single dose of 150 mg SIM/capsule (Olysio®) to healthy individuals. Conclusion: This method exhibits high sensitivity with a low limit of quantification 10 ng mL-1, good selectivity using fluorescence detection, wide linear application range 10-3000 ng mL-1, good recovery and highly precise and validation results. The developed method can be applied in routine analysis for real samples.

scholarly journals Rapid and Sensitive Method for Quantitative Determination of Lopinavir and Ritonavir in Human Plasma by Liquid Chromatography- Tandem Mass Specrtometry

2009 ◽  
Vol 6 (1) ◽  
pp. 223-230 ◽  
Author(s):  
G. A. Temghare ◽  
S. S. Shetye ◽  
S. S. Joshi
Keyword(s):  
Liquid Chromatography ◽  
Human Plasma ◽  
Solid Phase ◽  
Internal Standard ◽  
Therapeutic Monitoring ◽  
Tandem Mass ◽  
Limit Of Quantification ◽  
Liquid Chromatography Tandem Mass ◽  
Sensitive Method

A rapid and sensitive liquid chromatography-mass spectrometric (LC-MS-MS) method for the simultaneous determination of lopinavir and ritonavir in human plasma using abacavir as internal standard has been developed and validated. Sample preparation of plasma involved solid phase extraction. Detection was performed using an Applied Biosystems Sciex API 2000 Mass spectrometer. The assay of lopinavir and ritonavir was linear over the range of 50 ng mL-1to 20000 ng mL-1and 20 ng mL-1to 3000 ng mL-1 respectively with a precision of <15% and accuracy in the range of 85-115%. The limit of quantification in plasma for lopinavir and ritonavir was 50 ng mL-1and 20 ng mL-1respectively. The described method has the advantage of being rapid and easy and it could be applied in therapeutic monitoring of these drugs in human plasma

scholarly journals HPLC determination of ketamine, norketamine, and dehydronorketamine in plasma with a high-purity reversed-phase sorbent

1998 ◽  
Vol 44 (3) ◽  
pp. 560-564 ◽  
Author(s):  
Sébastien Bolze ◽  
Roselyne Boulieu
Keyword(s):  
Low Dose ◽  
Reversed Phase ◽  
Hplc Method ◽  
Pharmacokinetic Studies ◽  
Liquid Liquid Extraction ◽  
Extraction Separation ◽  
Acetate Mixture ◽  
New Stationary Phase ◽  
High Column

Abstract We developed an isocratic, selective, and very sensitive HPLC method for the determination of ketamine and its two main metabolites in plasma. The compounds were extracted from plasma by a liquid–liquid extraction with a dichloromethane:ethyl acetate mixture followed by an acidic back-extraction. Separation was achieved on a new stationary phase, Purospher RP-18 end-capped, with a mobile phase containing acetonitrile:0.03 mol/L phosphate buffer (23:77 by vol) adjusted to pH 7.2. Because of the high column efficiency and the significant improvement of peak symmetry, the quantification limit could be down to 5 μg/L for ketamine and norketamine (NK). The intraday and interday CVs ranged from 1.7% to 5.8% and 3.1% to 10.2% for all compounds respectively. The method is sensitive enough for monitoring ketamine, NK, and dehydroketamine in plasma during pharmacokinetic studies after an intravenous bolus of a low dose of ketamine.

Determination of Ibuprofen in Human Plasma and Urine by Gas Chromatography/Mass Spectrometry

2014 ◽  
Vol 97 (2) ◽  
pp. 415-420 ◽  
Author(s):  
Bilal Yilmaz ◽  
Ali Fuat Erdem
Keyword(s):  
Human Plasma ◽  
Internal Standard ◽  
Gas Chromatography Mass Spectrometry ◽  
Oral Tablet ◽  
Liquid Liquid Extraction ◽  
Human Plasma And Urine ◽  
The Mean ◽  
Interday Precision ◽  
Better Than

Abstract This paper describes a GC/MS method for the determination of ibuprofen in human plasma and urine. Ibuprofen and internal standard naproxen were extractedfrom plasma and urine by using a liquid–liquid extraction method. Derivatization was carried outusing N-methyl-N-(trimethylsilyl) trifluoroacetamide. Calibration curves were linear over the concentration range of 0.05–5.0 and 0.1–10.0 μg/mL for plasma and urine, respectively. Intraday and interday precision (RSD) values for ibuprofen in plasma and urine were less than 6.31%, and accuracy (relative error) was better than 12.00%. The mean recovery of ibuprofen was 89.53% for plasma and 93.73% for urine. TheLOD was 0.015 and 0.03 μg/mL and the LOQ was 0.05 and 0.1 μg/mL for plasma and urine, respectively. The method was successfully applied to blood samples from three healthy male volunteers who had been given an oral tablet of 600 mg ibuprofen.

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