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Visakhapatnam andhra Pradesh, India

Rao P.S.,Yalamarty Pharmacy College | Ghosh G.,Siksha O' Anusandhan University
Journal of Analytical Chemistry | Year: 2015

A novel liquid chromatography-tandem mass spectrometry (LC-MS-MS) method is described for the quantitative determination of diclofenac in human K2EDTA plasma in negative ion mode and validated using zidovudine as internal standard (IS). Sample preparation was accomplished by solid phase extraction technique. The eluted samples were chromatographed on Zorbax XDB phenyl column (75 × 4.6 mm, 3.5 μm) Agilent Technologies, using a mobile phase consisting of HPLC grade acetonitrile—0.2% acetic acid in HPLC water (80: 20, v/v).The injection volume was 15 μL and the total run time was 2.0 min. The method was validated over a linear concentration range of 25 to 4004 ng/mL diclofenac. The precursors to product ion transitions m/z 294.10 to 249.90 (diclofenac) and m/z 266.0 to 222.90 (zidovudine, IS) were used for quantitation. The retention times were 1.12 and 0.86 min for diclofenac and zidovudine, respectively. Validation results show that the method is selective and capable of quantifying the analyte with good precision and accuracy. The method is stable for the studied parameters. Therefore, a rapid, sensitive LC-MS-MS method for quantification of diclofenac in human plasma was developed and can be used in therapeutic drug monitoring of this drug. © 2015, Pleiades Publishing, Ltd. Source


Banerjee M.,Institute of Pharmacy and Technology | Sahoo N.K.,Yalamarty Pharmacy College
Asian Journal of Pharmaceutical and Clinical Research | Year: 2011

A simple, specific, accurate, cost effective & time efficient reversed phase high performance liquid chromatographic method was developed for the determination of Mesalamine, using RP-18 (4.6 mm X 2.5 cm) column and a mobile phase composed of methanol: water (50:50 v/v) at flow rate 0.5 ml/min. The retention time of Mesalamine was found to be 3.070 min which is much less than the other method used for the estimation of Mesalamine. Linearity was established for Mesalamine in the range 20-50 μg/ml. The percentage recovery of Mesalamine was found to be in the range 99.77%.The proposed method is precise, accurate, selective and rapid for the determination of Mesalamine for QC level. Source


Sahoo N.K.,Yalamarty Pharmacy College | Sahu M.,Yalamarty Pharmacy College | Rao P.S.,Yalamarty Pharmacy College | Ghosh G.,Siksha O' Anusandhan University
Asian Journal of Chemistry | Year: 2014

A novel liquid chromatography tandem mass spectrometry method is described for the quantitative determination of lornoxicam in human K2 EDTA plasma in positive ion mode and validated using piroxicam as internal standard according to linearity, selectivity, precision, recovery and various stability studies. Sample preparation was accomplished by liquid liquid extraction technique. The eluted samples were chromatographed on ACE C18 (150 × 4.6 mm, 5 μ) column (agilent technologies) using a mobile phase consisting of HPLC grade acetonitrile: 0.3 % formic acid buffer (80:20 v/v) with injection volume of 15 μL and a run time of 3 min. The precursor to product ion transitions m/z 372.10 to 121.10 (lornoxicam) and m/z 332.10 to 95.20 (piroxicam, IS) were used for quantization. The calibration graph of lornoxicam was linear with r2 > 0.990 over a concentration range of 5.086 ng/mL to 1518.325 ng/mL. CV % of intra- and inter-day precisions were found satisfactory and well within the limits. The drug was found to be stable for the studied parameters and found to be interference free for matrix effect with appreciable recovery. The novelty of the method makes it highly valuable, rapid, selective and sencitive for quantification of lornoxicam in human plasma and can be used in therapeutic drug monitoring of this drug. Source


Sahoo N.K.,Yalamarty Pharmacy College | Sahu M.,Yalamarty Pharmacy College | Rao P.S.,Yalamarty Pharmacy College | Ghosh G.,Siksha O' Anusandhan University
Tropical Journal of Pharmaceutical Research | Year: 2014

Purpose: To determine naproxen levels in human plasma using a new liquid chromatography-Mass spectroscopy/Mass spectroscopy (LC-MS/MS) method that involves a simple and single step extraction procedure using low-cost reagents.Conclusion: A rapid and selective LC-MS/MS method for the quantification of naproxen in human plasma has been developed and can be used in therapeutic drug monitoring of this drug as well as in bioequivalence studies of the drug.Method: A novel liquid chromatography–tandem mass spectrometry method for the quantitative determination of naproxen in human K2-EDTA plasma in negative ion mode was employed and validated using zidovudine as internal standard (IS). Sample preparation was accomplished by liquidliquid extraction technique. The eluted samples were chromatographed on Zorbax Eclipse XDB phenyl 4.6 × 75 mm, 3.5 μm column (Agilent Technologies) using a mobile phase consisting of acetonitrile: 20 mM ammonium acetate (90:10 v/v).The injection volume was 15 μL and the total run time was 3.0 min. The method was validated for all parameters for naproxen.Results: The method showed selectivity and linearity over a concentration range of 500.1 ng/mL to 100028.5 ng/mL The validation data indicate precision and accuracy of 90 -110% and < 15%), respectively, as well as recovery (80.63%), stability (mostly stable) and carryover (0%). © Pharmacotherapy Group, Faculty of Pharmacy, University of Benin, Benin City, 300001 Nigeria. All rights reserved. Source

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