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.

Development and Validation of a Liquid Chromatography/Mass Spectrometry Method for the Simultaneous Quantitation of Rosuvastatin and Ezetimibe in Human Plasma

2013 ◽  
Vol 96 (2) ◽  
pp. 307-312 ◽  
Author(s):  
Susheel John Varghese ◽  
Ravi Thengungal Kochupappy
Keyword(s):  
Human Plasma ◽  
Internal Standard ◽  
Liquid Chromatography Mass Spectrometry ◽  
Selected Ion Monitoring ◽  
Spectrometry Method ◽  
Esi Ms ◽  
Standard Curve ◽  
Liquid Liquid Extraction ◽  
Development And Validation

Abstract A simple, rapid, and sensitive LC/electrospray ionization (ESI)-MS method was developed and validated for the simultaneous determination of rosuvastatin (ROS) and ezetimibe (EZE) in human plasma. Following liquid–liquid extraction, the analytes and an internal standard, atorvastatin (ATO), were separated using an isocratic mobile phase comprising 0.1% (v/v) formic acid–methanol (20 + 80, v/v) on an RP-C18 column. Detection was performed on a mass spectrometer by selected ion monitoring using their respective [M-H]– ions, m/z 480 for ROS, m/z 408 for EZE, and m/z 557 for ATO. For both analytes, the method was linear in the range of 0.1 to 10 ng/mL. Acceptable precision and accuracy were obtained for concentrations over the standard curve range. A run time of 4 min made it possible to determine many plasma samples/day. The validated LC/ESI-MS method can be used to study pharmacokinetics, bioavailability, and bioequivalence of combined dosage forms of ROS and EZE.

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 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

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.

scholarly journals A Rapid and Selective LC-MS/MS Method for Quantification of Quetiapine in Human Plasma and its Application to Pharmacokinetic Study on Indian Schizophrenia Patients

2011 ◽  
Vol 8 (4) ◽  
pp. 1802-1814 ◽  
Author(s):  
S. Ravinder ◽  
A. T. Bapuji ◽  
K. Mukkanti ◽  
M. Nagesh ◽  
H. L. V. Ravikiran
Keyword(s):  
Mass Spectrometry ◽  
Human Plasma ◽  
Pharmacokinetic Study ◽  
Dynamic Range ◽  
Solid Phase ◽  
Multiple Reaction Monitoring ◽  
Internal Standard ◽  
Plasma Samples ◽  
Standard Curve ◽  
Multiple Reaction Monitoring Mode

A rapid, robust and selective high pressure liquid chromatography–positive electrospray ionization tandem mass spectrometry method has been developed and validated for the quantification of quetiapine (QUE) in human plasma with K2EDTA using oxcarbazepine (IS) as an internal standard. Analyte and internal standard were extracted from human plasma by solid-phase extraction using acetonitrile. The eluted samples were chromatographed on a C18 column by using a 10:75:15v/v mixture of ammonium formate buffer (5 mM, pH 4.50) and acetonitrile and methanol as an isocratic mobile phase at a flow rate of 0.4 mL/min and analyzed by mass spectrometry in the multiple reaction monitoring mode using the respective [M+H]+ions,m/z384.3/253.2 for Quetiapine andm/z253.1/208.1 for the internal standard. The assay exhibited a linear dynamic range of 5.01 - 2501.04 ng/mL for quetiapine in human plasma. Acceptable precision and accuracy were obtained for concentrations over the standard curve range. A run time of 2.5 min for each sample made it possible to analyze 300 patient plasma samples per day. The validated method has been successfully used for the estimation of quetiapine in real time schizophrenia patient’s plasma samples for pharmacokinetic study.

scholarly journals A Simple High-Performance Liquid Chromatography Method for Simultaneous Determination of Three Triazole Antifungals in Human Plasma

2012 ◽  
Vol 57 (1) ◽  
pp. 484-489 ◽  
Author(s):  
Mei Zhang ◽  
Grant A. Moore ◽  
Murray L. Barclay ◽  
Evan J. Begg
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
Simultaneous Determination ◽  
Human Plasma ◽  
High Performance ◽  
Internal Standard ◽  
Gradient Elution ◽  
Limit Of Quantification ◽  
Chromatography Method

ABSTRACTA rapid and simple high-performance liquid chromatography (HPLC) assay was developed for the simultaneous determination of three triazole antifungals (voriconazole, posaconazole, and itraconazole and the metabolite of itraconazole, hydroxyitraconazole) in human plasma. Sample preparation involved a simple one-step protein precipitation with 1.0 M perchloric acid and methanol. After centrifugation, the supernatant was injected directly into the HPLC system. Voriconazole, posaconazole, itraconazole, its metabolite hydroxyitraconazole, and the internal standard naproxen were resolved on a C6-phenyl column using gradient elution of 0.01 M phosphate buffer, pH 3.5, and acetonitrile and detected with UV detection at 262 nm. Standard curves were linear over the concentration range of 0.05 to 10 mg/liter (r2> 0.99). Bias was <8.0% from 0.05 to 10 mg/liter, intra- and interday coefficients of variation (imprecision) were <10%, and the limit of quantification was 0.05 mg/liter.

scholarly journals Simultaneous Determination of Ropivacaine and 3-Hydroxy Ropivacaine in Cerebrospinal Fluid by UPLC-MS/MS

2020 ◽  
Vol 2020 ◽  
pp. 1-6
Author(s):  
Siyuan Chen ◽  
Jianshe Ma ◽  
Xianqin Wang ◽  
Quan Zhou
Keyword(s):  
Cerebrospinal Fluid ◽  
Extraction Efficiency ◽  
Multiple Reaction Monitoring ◽  
Internal Standard ◽  
Reaction Monitoring ◽  
Limit Of Quantification ◽  
Liquid Liquid Extraction ◽  
The Matrix ◽  
Interday Precision

In this paper, a UPLC-MS/MS method was developed for the determination of ropivacaine and its metabolite 3-hydroxy ropivacaine in cerebrospinal fluid. The cerebrospinal fluid was processed by ethyl acetate liquid-liquid extraction. The multiple reaction monitoring (MRM) mode was used for quantitative analysis by monitoring the transitions of m/z 275.3 → 126.2 for ropivacaine, m/z 291.0 → 126.0 for 3-hydroxy ropivacaine, and m/z 290.2 → 198.2 for the internal standard. Standard curves for ropivacaine and 3-hydroxy ropivacaine in cerebrospinal fluid were conducted over the concentration range of 0.2–2000 ng/mL, demonstrating excellent linearity, and the lower limit of quantification was 0.2 ng/mL. The intraday precision of ropivacaine and 3-hydroxy ropivacaine was less than 11%, while the interday precision was less than 7%. The accuracy ranged between 87% and 107%, the average extraction efficiency was higher than 79%, and the matrix effect was between 89% and 98%. The developed method was then applied to a case of suspected poisoning of ropivacaine.

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