scholarly journals Quick and simple LC-MS/MS method for the determination of simvastatin in human plasma: application to pharmacokinetics and bioequivalence studies

2014 ◽  
Vol 50 (3) ◽  
pp. 543-550 ◽  
Author(s):  
Suéllen Cristina Rennó Silva ◽  
Gustavo Rodrigues de Rezende ◽  
Vanessa Bergamin Boralli
Keyword(s):  
Mass Spectrometry ◽  
Liquid Chromatography ◽  
Human Plasma ◽  
Multiple Reaction Monitoring ◽  
Internal Standard ◽  
Methyl Tert Butyl Ether ◽  
Ionization Mass ◽  
Butyl Ether ◽  
Relative Standard

A simple, rapid, and sensitive method based on liquid chromatography-tandem mass spectrometry for the quantitative determination of simvastatin in human plasma was developed and validated. After a simple extraction with methyl tert-butyl ether, the analyte and internal standard (lovastatin) were analyzed using reverse-phase liquid chromatography, on a Kinetex C18column (100 × 4.6 mm, 2.6 μm) using acetonitrile: ammonium acetate (2 mM + 0.025 % formic acid) (70: 30, v/v) as a mobile phase in a run time of 3.5 min. Detection was carried out using electrospray positive ionization mass spectrometry in the multiple-reaction monitoring mode. The method was linear over 0.04-40.0 ng/mL concentration range. The mean extraction recovery of simvastatin was 82% (RSD within 15%). Intraday and interday precisions (as relative standard deviation) were all ≤8,7% with accuracy (as relative error) of ±8%. This rapid and reliable method was successfully applied for a bioequivalence study of 40 mg of simvastatin orally disintegrating tablets in 44 healthy volunteers, showing that this method is suitable for the quantification of simvastatin in human plasma samples for pharmacokinetics and bioequivalence studies.

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>

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 Sensitive LC-MS/MS Method for the Simultaneous Determination of Bisoprolol and Triamterene in human plasma

2017 ◽  
Vol 10 (4) ◽  
pp. 341
Author(s):  
Hemavathi G ◽  
Hipparagi S M
Keyword(s):  
Mass Spectrometry ◽  
Liquid Chromatography ◽  
Simultaneous Determination ◽  
Human Plasma ◽  
Internal Standard ◽  
Ionization Mass ◽  
Highly Sensitive ◽  
Plasma Pharmacokinetics ◽  
Mass Spectrometry Mass Spectrometry

Objective: A highly sensitive, specific, and rapid liquid chromatography-electrospray ionization-mass spectrometry (MS)/MS method has been developed and validated for the simultaneous quantification of bisoprolol and triamterene in human plasma using metoprolol as an internal standard (IS) as per regulatory guidelines.Methods: Both the analytes and IS were extracted from plasma using a protein precipitation extraction method. Chromatography was achieved on Welchrom XB C18, 50 mm×4.6 mm, 5 µm column using an isocratic mobile phase (2 mM ammonium formate acetonitrile, 70:30 v/v) at a flow rate of 0.60 ml/minute.Results: The total chromatographic run time was 3.5 minute and the elution of bisoprolol, triamterene, and IS occurred at ~2.57, 1.30 and 1.57 minute, respectively. A linear response function was established at 2.04-210 ng/ml for both the analytes in human plasma. The intra- and inter-day accuracy and precisions were in the range of 1.12-7.87 and 1.26-6.36%; 1.46-6.13 and 1.65-7.34% for bisoprolol and triamterene, respectively.Conclusion: A new robust method was developed for simultaneous determination of Bisoprolol and Triamterene in human plasma. The method was strictly validated according to the ICH [1] guidelines. The information thus obtained from the study can be used for the full pharmacokinetic profiling in individuals.Keywords: Bisoprolol, Triamterene, Liquid chromatography-mass spectrometry/mass spectrometry, Method validation, Human plasma,Pharmacokinetics.

Determination of a Yellow Rice Toxin, Luteoskyrin, in Rice by Using Liquid Chromatography–Tandem Mass Spectrometry with Electrospray Ionization

2009 ◽  
Vol 72 (6) ◽  
pp. 1321-1326 ◽  
Author(s):  
KOHEI MIZUTANI ◽  
SUSUMU KUMAGAI ◽  
NAOKI MOCHIZUKI ◽  
YASUSHI KITAGAWA ◽  
YOSHIKO SUGITA-KONISHI
Keyword(s):  
Mass Spectrometry ◽  
Liquid Chromatography ◽  
Electrospray Ionization ◽  
High Performance ◽  
Solid Phase ◽  
Multiple Reaction Monitoring ◽  
Phase System ◽  
Ionization Mass ◽  
Solid Phase Extraction Cartridge ◽  
Relative Standard

Penicillium islandicum produces luteoskyrin (LUT), a yellow rice toxin that has been found frequently in rice. However, conventional analytical methods for determining LUT are limited, are complicated, and exhibit low sensitivity. In this study, an analytical method more sensitive and simple based on high-performance liquid chromatography combined with electrospray ionization mass spectrometry was developed. The cleanup procedure of the method was one step, using a solid-phase extraction cartridge. An isocratic mobile-phase system, consisting of acetonitrile–water–acetic acid (50:49:1 [vol/vol/vol]) at a flow rate of 0.2 ml/min, was utilized to obtain the best resolution. Our method showed good linearity (r = 0.9993, 0.5 to 50 ng/g) and high repeatability (relative standard deviation = 8.9 and 5.1% at levels of 0.5 and 10 ng/g, respectively) in the fortification test. The detection and quantification limits for the method in multiple-reaction monitoring mode were 0.1 and 0.3 ng/g, respectively. The average recovery of LUT in spiked rice at 0.5 and 10 ng/g was 80.7 and 85.2%, respectively. The method developed in this study should be applicable to survey LUT in rice, with high sensitivity, selectivity, and rapidity.

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