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 SIMULTANEOUS ESTIMATION OF PROPAFENONE AND ITS TWO METABOLITES IN HUMAN PLASMA BY LIQUID CHROMATOGRAPHY/TANDEM MASS SPECTROMETRY LC-MS/MS

2017 ◽  
Vol 9 (8) ◽  
pp. 192
Author(s):  
Rajeev Kumar Gupta ◽  
Anand Chaurasia ◽  
Brijeshkunvar Mishra
Keyword(s):  
Mass Spectrometry ◽  
Liquid Chromatography ◽  
Tandem Mass Spectrometry ◽  
Human Plasma ◽  
Dynamic Range ◽  
Multiple Reaction Monitoring ◽  
Internal Standard ◽  
Simultaneous Estimation ◽  
Tandem Mass ◽  
Plasma Samples

Objective: A simple, sensitive and rapid performance liquid chromatography/positive ion electrospray tandem mass spectrometry method was to be developed and validated for quantification of propafenone (PPF) and its two major metabolite 5-hydroxy propafenone (5-OHP) and N-depropyl propafenone (NDP) in human plasma.Methods: Liquid-liquid extraction (LLE) with ethyl acetate was used of extraction of plasma samples. The analytes were separated using an isocratic mixture of 0.1% formic acid/acetonitrile (20:80 v/v) on a reversed-phase column Hypurity Advance C18 50 x2.1 mm, 5µ and analysed by mass spectrometry in the multiple reaction monitoring mode using the respective [M+H] Ions. The m/z was 342.20/116.10 for propafenone, m/z 299.80/74.10 for N depropyl propafenone and m/z 358.30/98.10 for 5-hydroxy propfenone along with m/z 409.2/238.0 for Amlodipine as internal standard respectively.Results: The method had a short chromatographic run time of 1.5 min. The method exhibited a linear dynamic range over 5.11 to 1000.73 ng/ml for propafenone, 0.51 to 100.06 ng/ml for N-depropyl propafenone and 5.11 to 1001.64 ng/ml for 5-hydroxy propafenone respectively, in human plasma.Conclusion: The validated method has been successfully used to analyze human plasma samples for application in pharmacokinetics, bioavailability and bioequivalence studies.

scholarly journals A RAPID AND SENSITIVE LIQUID CHROMATOGRAPHY- MASS SPECTROMETRY/MASS SPECTROMETRY METHOD FOR ESTIMATION OF PIOGLITAZONE, KETO PIOGLITAZONE AND HYDROXY PIOGLITAZONE IN HUMAN PLASMA

2017 ◽  
Vol 10 (12) ◽  
pp. 120
Author(s):  
Revathi Naga Lakshmi Ponnuri ◽  
Prahlad Pragallapati ◽  
Ravindra N ◽  
Venkata Basaveswara Rao Mandava
Keyword(s):  
Mass Spectrometry ◽  
Liquid Chromatography ◽  
Human Plasma ◽  
Multiple Reaction Monitoring ◽  
Internal Standard ◽  
Pharmacokinetic Parameters ◽  
Validation Parameters ◽  
Liquid Chromatography Tandem Mass ◽  
Multiple Reaction Monitoring Mode

  Objective: The main objective of the work was to develop a straightforward, fast and selective liquid chromatography/tandem mass spectrometry (LC-MS/MS) assay for determination of pioglitazone (PG), keto pioglitazone (KPG), and hydroxy pioglitazone (HPG) in human plasma and to validate as per recent guidelines.Methods: Analyte and the internal standard (IS) were extracted from plasma through liquid-liquid extraction and chromatographed on a Xterra RP18, 100×4.6, 5 μ column using methanol: acetonitrile mixture and 10 mM Ammonium formate buffer (70:30, v/v) as the mobile phase at a flow rate of 0.7 mL/min. The API-3200 Q Trap LC-MS/MS instrument in multiple reaction monitoring mode was used for detection. Diphenhydramine was utilized as IS.Results: The linearity was established in the concentration range of 20.15-1007.58 ng/mL for PG, 20.35-1017.58 ng/mL for KPG, and 19.68-491.22 ng/mL for HPG in human plasma. All the validation parameters were well within the acceptance limits.Conclusion: A new simple LC-MS/MS method was developed for the determination of PG, KPG, and HPG in human plasma. This method can be easily applied for the estimation of pharmacokinetic parameters of PG, KPG, and HPG.

scholarly journals LC-MS/MS determination of glimepiride in human plasma with a high recovery at picogram scale: Pharmacokinetic study after oral administration

2020 ◽  
Author(s):  
Ahmed K. Kammoun ◽  
Zuhier Ahmed Awan ◽  
Tarek Elawady ◽  
Alaa Khedr ◽  
Mohamed I. El-Awady
Keyword(s):  
Oral Administration ◽  
Human Plasma ◽  
Pharmacokinetic Study ◽  
Methylene Chloride ◽  
Limit Of Detection ◽  
Solid Phase ◽  
Multiple Reaction Monitoring ◽  
Internal Standard ◽  
Range Limit ◽  
Extraction Recovery

AbstractAlthough glimepiride (GLM) is the first-line treatment of Type II diabetes, low extraction recovery is still a significant limitation in previous plasma analysis methods. An optimized solid-phase extraction method of GLM in human plasma with excellent extraction recovery, 100 ± 0.06%, was achieved using liquid chromatography-electrospray ionization tandem mass spectrometry and Gliclazide (GLZ) as an internal standard. GLM was extracted from 100 µL plasma sample using Sep-Pak® vac 1cc (100 mg) C18 column and methylene chloride: methanol (2: 1, v/v) as eluant. Both GLM and GLZ were monitored by a triple quad mass spectrometer applying positive multiple reaction monitoring mode (+MRM). The protonated precursor ions and product ions of GLM and GLZ were m/z 491(352), and m/z 324 (127), respectively. The detection and measurement of low levels of GLM in human plasma reached to picogram range (limit of detection (LOD) = 60 pg/mL, limit of quantification (LOQ) = 200 pg/mL). The method was validated in terms of selectivity, linearity, recovery, accuracy, and precision. The method was successfully applied to the pharmacokinetic study of GLM following oral administration of 1 mg GLM tablets to 12 healthy volunteers.

A Rapid and Sensitive Method for the Pharmacokinetic Study of Janumet (Sitagliptin and Metformin) Tablets by LC-MS/MS Coupled with Ion-Pair Solid Phase Extraction

2019 ◽  
Vol 15 (7) ◽  
pp. 776-784
Author(s):  
Xiaonian Han ◽  
Jing Wang ◽  
Jing Huang ◽  
Lirong Peng
Keyword(s):  
Solid Phase Extraction ◽  
Pharmacokinetic Study ◽  
Solid Phase ◽  
Multiple Reaction Monitoring ◽  
Ion Pair ◽  
Phase Extraction ◽  
Plasma Samples ◽  
Ionization Source ◽  
Tandem Mass Spectrometric

Background: As first-line treatments for diabetes, sitagliptin and metformin have been widely prescribed as a combination to enhance the therapeutic effect. Objective: To establish a methodology to simultaneously monitor the two drugs in vivo by a reversedphase Liquid Chromatography-Tandem Mass Spectrometric (LC-MS/MS) method. Methods: The two drugs were extracted from 50 μl human plasma by ion-pair solid phase extraction. The separation of the plasma samples was implemented on an Agilent Zorbax SB-CN column (150×4.6 mm, 5.0 µm). The mobile phase was the mixture (80:20, v/v) of methanol and 5.0 mM ammonium formate in water (pH 4.5). An ion trap spectrometer equipped with an electrospray ionization source was utilized to detect the elution in positive mode. Quantification of the analytes was achieved by Multiple Reaction Monitoring (MRM) using the transitions of m/z 408.3→235.1 for sitagliptin and m/z 130.1→ 60.2 for metformin. Results: Sitagliptin and metformin demonstrated good linearity among the range of 1.00-1000 ng/mL and 5.00-4000 ng/mL. The intra-day and inter-day investigations displayed precisions of ≤ 3.6% and an accuracy range of -7.5% to 6.0% for the two drugs. The mean recovery of the two drugs was 96.0% and 98.5%. Under mandatory storage conditions, both the drugs gave an acceptable stability. The throughput of the assay was found to be more than 100 plasma samples per day ascribed to the run time of 3.0 min for each sample. Conclusion: The developed method was successfully applied to a pharmacokinetic study for a fixeddose tablet formulation containing 50 mg sitagliptin and 500 mg metformin in 12 healthy volunteers.

scholarly journals NEW METHOD DEVELOPMENT AND VALIDATION FOR THE DETERMINATION OF FEBUXOSTAT IN HUMAN PLASMA BY LIQUID CHROMATOGRAPHY–MASS SPECTROMETRY

2016 ◽  
Vol 8 (9) ◽  
pp. 61 ◽  
Author(s):  
Narottam Pal ◽  
Avanapu Srinivasa Rao ◽  
Pigilli Ravikumar
Keyword(s):  
Mass Spectrometry ◽  
Liquid Chromatography ◽  
Human Plasma ◽  
Method Development ◽  
Multiple Reaction Monitoring ◽  
Internal Standard ◽  
New Method ◽  
Liquid Chromatography Mass Spectrometry ◽  
Chromatography Mass Spectrometry

<p><strong>Objective</strong>:<strong> </strong>To develop a new method and validate the same for the determination of Febuxostat (FBS) in human plasma by liquid chromatography–mass spectrometry (LCMS).</p><p><strong>Methods</strong>:<strong> </strong>The present method utilized reversed-phase high-performance liquid chromatography with tandem mass spectroscopy. Febuxostat D9 (FBS D9) was used as internal standard (IS). The analyte and internal standard were separated from human plasma by using solid phase extraction method. Zorbax Eclipse XDB, C<sub>8</sub>, 100 mm x 4.6 mm, 3.5 µm column was used and HPLC grade acetonitrile, 5 millimolar (mM) ammonium format (80: 20, v/v) as mobile phase, detected by mass spectrometry operating in positive ion and multiple reaction monitoring modes.</p><p><strong>Results</strong>:<strong> </strong>The parent and production transitions for FBS and internal standard were at m/z 317.1→261.0 and 326.1→262.0 respectively. The method was validated for system suitability, specificity, carryover effect, linearity, precision, accuracy, matrix effect, sensitivity and stability. The linearity range was from 20.131 ng/ml to10015. 534 ng/ml with a correlation coefficient of 0.999. Precision results (%CV) across six quality control samples were within the limit. The percentage recovery of FBS and internal standard from matrix samples was found to be 76.57% and 75.03% respectively.</p><p><strong>Conclusion</strong>:<strong> </strong>Present study describes new LC-MS method for the quantification of FBS in a pharmaceutical formulation. According to validation results, it was found to be a simple, sensitive, accurate and precise method and also free from any kind of interference. Therefore the proposed analytical method can be used for routine analysis for the estimation of FBS in its formulation.</p>

Development and validation of bioanalytical liquid chromatography–tandem mass spectrometry method for the estimation of pentoxifylline in human plasma: Application for a comparative pharmacokinetic study

2018 ◽  
Vol 25 (4) ◽  
pp. 372-380 ◽  
Author(s):  
Sireesha Dodda ◽  
Ajitha Makula ◽  
Srinivasa R Polagani ◽  
Raj N Kandhagatla
Keyword(s):  
Mass Spectrometry ◽  
Liquid Chromatography ◽  
Tandem Mass Spectrometry ◽  
Human Plasma ◽  
Pharmacokinetic Study ◽  
Internal Standard ◽  
Tandem Mass ◽  
Comparative Pharmacokinetic ◽  
Chromatography Tandem Mass Spectrometry ◽  
Liquid Chromatography Tandem Mass

A method for bioanalysis of pentoxifylline in human plasma was developed using liquid chromatography–tandem mass spectrometry, which is simple, specific, and sensitive. Pentoxifylline D5 was used as the internal standard. Employing only 100 µl of human plasma, processing was done with solid-phase extraction technique. The analyte and the internal standard were separated from endogenous components on Ace phenyl column using a mixture of 5 mM ammonium acetate buffer and high performance liquid chromatography grade acetonitrile (60:40, v/v) as mobile phase at a flow rate of 1 ml/min. The linearity of the method was in the range of 3–1200 ng/ml with r2 > 0.99. Positive ion MRM mode was used for the detection of the analyte and the internal standard. The method was validated as per the US Food and Drug Administration guidelines and the results were within the acceptance limits. The proposed method was applied for comparative pharmacokinetic study of pentoxifylline after oral administration of 400 and 600 mg tablets to South Indian male subjects under fed conditions.

scholarly journals ANALYTICAL METHOD DEVELOPMENT AND VALIDATION OF AMLODIPINE IN HUMAN PLASMA USING LIQUID CHROMATOGRAPHY-MASS SPECTROMETRY/MASS SPECTROMETRY

2018 ◽  
Vol 11 (7) ◽  
pp. 393
Author(s):  
Akiful Haque M ◽  
Shanthi Priya D K ◽  
Dibyalochan Mohanty ◽  
Vasudha Bakshi ◽  
Narender Boggula
Keyword(s):  
Mass Spectrometry ◽  
Human Plasma ◽  
Analytical Method ◽  
High Performance ◽  
Method Development ◽  
Solid Phase ◽  
Internal Standard ◽  
High Performance Liquid Chromatographic ◽  
Economic Method ◽  
Positive Ion

Objective: The objective of the present investigation was to develop a novel, simple, and economic method for the estimation of amlodipine in positive ion mode in human plasma using amlodipine maleate d4 as an internal standard.Methods: The chromatographic separation was performed on Zorbax SB, C18, 50 mm*4.6 mm, and 3.5 mm. The mobile phase was prepared with a mixture of 5 mm ammonium acetate in 0.1% formic acid: High performance liquid chromatographic (HPLC) grade methanol:HPLC grade acetonitrile (40:30:30) that run isocratically at the flow rate of 0.700 ml/min and run time at 2.50 min.Results: The analytical method is valid for the estimation of amlodipine, in human plasma over a range of 0.100 ng/ml–9.990 ng/ml with the detection of amlodipine m/z - 409.10 (parent) and 238.00 (product), and internal standard Amlodipine Maleate d4 m/z - 413.20 (parent), and 238.00 (product) in positive ion mode. The results of carryover test, matrix effect, linearity, precision and accuracy, stabilities, dilution integrity, and run size evaluation test presented in this report are within the acceptance range.Conclusion: A sensitive method for the separation and determination of amlodipine in plasma has been developed based on solid-phase extraction with disposable extraction cartridges in combination with LC and mass spectrophotometers (MS/MS).

scholarly journals Bioanalytical Method Development and Validation of Memantine in Human Plasma by High Performance Liquid Chromatography with Tandem Mass Spectrometry: Application to Bioequivalence Study

2012 ◽  
Vol 2012 ◽  
pp. 1-8 ◽  
Author(s):  
Ravi Kumar Konda ◽  
B. R. Challa ◽  
Babu Rao Chandu ◽  
Kothapalli B. Chandrasekhar
Keyword(s):  
Human Plasma ◽  
High Performance ◽  
Method Development ◽  
Dynamic Range ◽  
Quantitative Estimation ◽  
Multiple Reaction Monitoring ◽  
Internal Standard ◽  
Bioequivalence Study ◽  
Healthy Human ◽  
Development And Validation

A simple, sensitive, and rapid HPLC-MS/MS method was developed and validated for quantitative estimation of memantine in human plasma. Chromatography was performed on Zorbax SB-C18(4.6×75 mm, 3.5 μm) column. Memantine (ME) and internal standard Memantine-d6(MED6) were extracted by using liquid-liquid extraction and analyzed by LC-ESI-MS/MS using multiple-reaction monitoring (MRM) mode. The assay exhibited a linear dynamic range of 50.00–50000.00 pg/ml for ME in human plasma. This method demonstrated an intra- and interday precision within the range of 2.1–3.7 and 1.4–7.8%, respectively. Further intra- and interday accuracy was within the range of 95.6–99.8 and 95.7–99.1% correspondingly. The mean recovery of ME and MED6 was86.07±6.87and80.31±5.70%, respectively. The described method was successfully employed in bioequivalence study of ME in Indian male healthy human volunteers under fasting conditions.

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.

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