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High performance liquid chromatography mass spectrometric method for the simultaneous quantification of pravastatin and aspirin in human plasma:Pharmacokinetic application

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Journal of Pharmaceutical Analysis 2012年第3期2卷 206-213页

作者： Srinivasa rao Polagani nageswara rao pilli Venkateswarlu Gandu Research Studies Rayalaseema UniversityKurnool 518002India University College of Pharmaceutical Sciences Jawaharlal Nehru Technological UniversityKukatpallyHyderabad 500085India Department of Chemistry Nizam CollegeOsmania UniversityHyderabad 500001India

A rapid and sensitive liquid chromatography-tandem mass spectrometric（LC-MS/MS） assay method has been developed and fully validated for the simultaneous quantification of pravastatin and aspirin in human *** was used as an internal *** and the internal standard were extracted from human plasma by liquid-liquid extraction technique using methyl tertiary butyl *** reconstituted samples were chromatographed on a Zorbax SB-C;8 column by using a mixture of 5 mM ammonium acetate buffer and acetonitrile（20:80,v/v） as the mobile phase at a flow rate of 0.8 mL/*** calibration curve obtained was linear（r≥0.99） over the concentration range of 0.50-600.29 ng/mL for pravastatin and 20.07-2012.00 ng/mL for *** validation was performed as per FDA guidelines and the results met the acceptance criteria.A run time of 2.0 min for each sample made it possible to analyze more than 400 human plasma samples per *** proposed method was found to be applicable to clinical studies.

关键词： Pravastatin Aspirin Human plasma Liquid-liquid extraction LC-MS/MS Pharmacokinetics

Simultaneous determination of atorvastatin,metformin and glimepiride in human plasma by LC-MS/MS and its application to a human pharmacokinetic study

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Journal of Pharmaceutical Analysis 2013年第1期3卷 9-19页

作者： Srinivasa rao Polagani nageswara rao pilli Ramakrishna Gajula Venkateswarlu Gandu Research Studies Rayalaseema University Wellquest Clinical Research Department of Chemistry Nizam CollegeOsmania University

A simple, rapid and sensitive liquid chromatography-tandem mass spectrometric （LC MS/ MS） assay method has been developed and fully validated for the simultaneous quantification of atorvastatin, metformin and g.）imepiride in human plasma. Carbamazepine was used as internal standard （IS）. The analytes were extracted from 200 μL aliquots of human plasma via protein precipitation using acetonitrile, The reconstituted samples were chromatographed on a Alltima HP C18 column by using a 60：40 （v/v） mixture of acetonitrile and 10 mM ammonium acetate （pH 3.0） as the mobile phase at a flow rate of 1.1 mL/min. The calibration curves obtained were linear （r2〉0.99） over the concentration range of 0.50-150.03 ng/mL for atorvastatin, 12.14-1207.50 ng/mL for metformin and 4.98-494.29 ng/mL for glimepiride. The API-4000 LC-MS/MS in multiple reaction monitoring （MRM） mode was used for detection. The results of the intra- and inter-day precision and accuracy studies were well within the acceptable limits. All the analytes were found to be stable in a battery of stability studies. The method is precise and sensitive enough for its intended purpose. A run time of 2.5 rain for each sample made it possible to analyze more than 300 plasma samples per day. The developed assay method was successfully applied to a pharmacokinetic study in human male volunteers.

关键词： Atorvastatin Metformin Glimepiride LC-MS/MS Human plasma Pharmacokinetics

A rapid and sensitive liquid chromatography-tandem mass spectrometric assay for duloxetine in human plasma:Its pharmacokinetic application

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Journal of Pharmaceutical Analysis 2013年第1期3卷 36-44页

作者： Ramakrishna Gajula Rambabu Maddela Vasu Babu Ravi Jaswanth Kumar Inamadugu nageswara rao pilli Wellquest Clinical Research Laboratories

This paper describes a simple, rapid and sensitive liquid chromatography tandem mass spectrometry assay for the determination of duloxetine in human plasma. A duloxetine stable labeled isotope （duloxetine ds） was used as an internal standard. Analyte and the internal standard were extracted from 100 btL of human plasma via solid phase extraction technique using Oasis HLB cartridges. The chromatographic separation was achieved on a Cl8 column by using a mixture of acetonitrile 5 mM ammonium acetate buffer （83：17, v/v） as the mobile phase at a flow rate of 0.9 mL/min. The calibration curve obtained was linear （r2≥0.99） over the concentration range of 0.05 101 ng/mL. Multiple-reaction monitoring mode （MRM） was used for quantification of ion transitions at rn/z 298.3/154.1 and 303.3/159.1 for the drug and the internal standard, respectively. Method validation was performed as per FDA guidelines and the results met the acceptance criteria. A run time of 2.5 min for each sample made it possible to analyze more than 300 plasma samples per day. The proposed method was found to be applicable to clinical studies.

关键词： Duloxetine in humanplasma Solid-phase extraction(SPE) Liquidchromatography-tandem mass spectro-metry Method validation Pharmacokinetic studies

Simultaneous determination of telmisartan and amlodipine in human plasma by LC-MS/MS and its application in a human pharmacokinetic study

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Journal of Pharmaceutical Analysis 2012年第5期2卷 319-326页

作者： Vasu Babu Ravi Jaswanth Kumar Inamadugu nageswara rao pilli Vudagandla Sreenivasulu Venkateswarlu Ponneri Research Studies Rayalaseema UniversityKurnool 518002India Wellquest Clinical Research Laboratories RamanthapurHyderabad 500013India BioPolymer and Thermophysical Lab Department of ChemistrySri Venkateswara UniversityTirupati 517502India Analytical and Environmental Chemistry Division Department of ChemistrySri Venkateswara UniversityTirupati 517502India

A rapid and sensitive liquid chromatography-tandem mass spectrometric （LC-MS/MS） assay method has been developed and fully validated for the simultaneous quantification of telmisartan and amlodipine in human plasma. Carbamazepine was used as an internal standard. Analytes and the internal standard were extracted from human plasma by solid-phase extraction technique using Waters Oasis HLB 1 cm3 （30 mg） extraction cartridge. The reconstituted samples were chromatographed on a Hypurity advance C18 column （50mm × 4.6mm, 5 gm） using a mixture of acetonitrile -5 mM ammonium acetate buffer （pH-4.0）（50：50, v/v） as the mobile phase at a flow rate of 0.8mL/min. The calibration curve obtained was linear （r_〉0.99） over the concentration range of 2.01-400.06 ng/mL for telmisartan and 0.05 -10.01 ng/mL for amlodipine. Method validation was performed as per FDA guidelines and the results met the acceptance criteria. A run time of 2.5 min for each sample made it possible to analyze more than 400 human plasma samples per day. The proposed method was found to be applicable to clinical studies.

关键词： Telmisartan Amlodipine Human plasma Solid-phase extraction LC-MS/MS Pharmacokinetics

Simultaneous determination of pioglitazone and candesartan in human plasma by LC-MS/MS and its application to a human pharmacokinetic study

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Journal of Pharmaceutical Analysis 2012年第3期2卷 167-173页

作者： Vijaya Kumari Karra nageswara rao pilli Jaswanth Kumar Inamadugu J.V.L.N.Seshagiri rao University College of Pharmaceutical Sciences Jawaharlal Nehru Technological UniversityKukatpallyHyderabad-500085India Analytical and Environmental Chemistry Division Department of ChemistrySri Venkateswara UniversityTirupati-517502India College of Pharmaceutical Sciences Andhra UniversityVisakhapatnam-530003India

A simple and rapid liquid chromatography-tandem mass spectrometric(LC-MS/MS) assay method has been developed and fully validated for simultaneous quantification of pioglitazone and candesartan in human *** was used as an internal *** analytes were extracted from human plasma samples by solid-phase extraction technique using a Strata-X 33 mm polymeric *** reconstituted samples were chromatographed on a C18 column by using a 80:20(v/v) mixture of acetonitrile and 0.1% formic acid as the mobile phase at a flow rate of 0.8 mL/*** calibration curves obtained were linear(rZ0.99) over the concentration range of 15-3000 ng/mL for pioglitazone and 5-608 ng/mL for *** results of the intra-and inter-day precision and accuracy studies were well within the acceptable limits.A run time of 2.7 min for each sample made it possible to analyze more than 300 plasma samples per *** proposed method was found to be applicable to clinical studies.

关键词： Pioglitazone Candesartan Human plasma Solid-phase extraction LC-MS/MS Pharmacokinetics

Simultaneous quantitation of lamivudine,zidovudine and nevirapine in human plasma by liquid chromatography-tandem mass spectrometry and application to a pharmacokinetic study

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Acta Pharmaceutica Sinica B 2012年第5期2卷 472-480页

作者： Murali Krishna Matta nageswara rao pilli Jaswanth Kumar Inamadugu Laxminarayana Burugula Seshagiri rao JVLN College of Pharmaceutical Sciences Jawaharlal Nehru Technological UniversityKukatpallyHyderabad 500085India Analytical and Environmental Chemistry Division Department of ChemistrySri Venkateswara UniversityTirupati 517502India College of Pharmaceutical Sciences Andhra UniversityVisakhapatnam 530003India

A rapid and sensitive LC-MS/MS method for the simultaneous quantitation of lamivudine,zidovudine and nevirapine in human plasma using abacavir as internal standard has been developed and *** analytes and IS were extracted from plasma by solid phase extraction using Oasis HLB cartridges and separated on a Hypurity Advance C18 column using a mixture of acetonitrile:0.1% formic acid(76:24,v/v)at a flow rate of 0.8 mL/*** involved an API-4000 LC MS/MS with electrospray ionization in the positive ion mode and multiple-reaction monitoring for *** method was validated according to FDA guidelines and shown to provide intra-and inter-day precision and accuracy within acceptable limits in a run time of only 3.5 *** method was sucessfully applied to a pharmacokinetic study involving a single oral administration of a combination tablet to human male volunteers.

关键词： Lamivudine Zidovudine Nevirapine Solid phase extraction LC-MS/MS Pharmacokinetics

Effect of pulsed current micro plasma arc welding process parameters on fusion zone grain size and ultimate tensile strength of Inconel 625 sheets

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Acta Metallurgica Sinica(English Letters) 2012年第3期25卷 179-189页

作者： Kondapalli Siva Prasad Chalamalasetti Srinivasa rao Damera nageswara rao Department of Mechanical Engineering Anil Neerukonda Institute of Technology & SciencesVisakha- patnam India Department of Mechanical Engineering AU College of Engineering Andhra UniversityVisakhapat- nam India Centurion University of Technology & Management Odisha India

The paper focuses on developing mathematical models to predict grain size and ul- timate tensile strength of pulsed current micro plasma arc welded Inconel 625 nickel alloy. Four factors, five levels, central composite rotatable design matrix is used to op- timize the number of experiments. The mathematical models have been developed by response surface method. The adequacy of the models is checked by analysis of vari- ance technique. By using the developed mathematical models, grain size and ultimate tensile strength of the joints can be predicted with 99% confidence level. Contour plots are drawn to study the interaction effect of pulsed current micro plasma arc welding parameters on fusion zone grain size and ultimate tensile strength of Inconel 625 weld joints.

关键词： Pulsed current Micro plasma arc welding ANOYA Response surface method: Inconel 625

Effect of Post Cryorolling Treatments on Microstructural and Mechanical Behaviour of Ultrafine Grained Al-Mg-Si Alloy

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Journal of Materials Science & Technology 2014年第10期30卷 998-1005页

作者： P.nageswara rao Dharmendra Singh R.Jayaganthan Department of Metallurgical and Materials Engineering Indian Institute of Technology Roorkee

To investigate the effect of post cryorolling treatments on simultaneous enhancement in strength and ductility of ultrafine grained material （UFG）, AI 6061 alloy was subjected to cryorolling followed by warm rolling （CR ＋ WR） and compared with cryorolling followed by short annealing （CR ＋ SA） at the same temperature. Transmission electron microscopy （TEM） was used to characterize the microstructural features of the processed material. The mechanical properties were investigated through Vickers hardness testing and tensile testing at room temperature. TEM, X-ray diffraction （XRD） and differential scanning calorimetry （DSC） were used to investigate the precipitation evolution in UFG material. Results indicated that the alloy subjected to CR ＋ WR has shown improved mechanical properties （114 HV, ultimate tensile strength （UTS）： 350 MPa） as compared to that in the case of CR ＋ SA （105 HV, UTS： 285 MPa）. The size of the precipitates observed in CR ＋ WR sample after peak ageing treatment is finer than that of peak aged CR ＋ SA sample. The UTS of peak aged CR ＋ WR sample （UTS： 390 MPa） was found to be higher than that of peak aged CR ＋ SA sample （UTS： 355 MPa）, without decrease in ductility.

关键词： Aluminium alloy Cryorolling Warm rolling Short annealing Mechanical properties Differential scanning calorimetry (DSC)

The Role of Vanadia for the Selective Oxidation of Benzyl Alcohol over Heteropolymolybdate Supported on Alumina

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催化学报 2011年第11期32卷 1719-1726页

作者： Pasupulet Siva nageswara rao Kasanneni Tirumala Venkateswara rao Potharaju S. SAI PRASAD Nakka LINGAIAH Catalysis Laboratory Inorganic and Physical Chemistty Division Indian Institute of Chemical Technology Hyderabad 500 607 lndia

A series of 12-molybdophosphoric acid (MPA) supported on V2O5 dispersed γ-Al2O3 catalysts with different vanadia loadings were prepared by impregnation and characterized by N2 adsorption-desorption, X-ray diffraction, temperature-programmed reduction, in situ laser Raman spectroscopy, UV-Vis diffused reflectance spectroscopy, scanning electron microscopy, and temperature-programmed desorption of NH3 techniques. Their catalytic activities were evaluated for the vapor phase aerobic oxidation of benzyl alcohol. The catalysts exhibited high catalytic activity and the conversion of benzyl alcohol depended on the vanadia content while the catalyst with 15 wt% V2O5 content showed optimum activity. The characterization results suggest the presence of well-dispersed V2O5 and partially disintegrated Keggin ions of MPA on the support. In situ Raman studies showed a reduced Mo(IV) species when the catalysts were calcined at high temperatures. The high oxidation activity of the catalysts is related to the synergistic effect between MPA and V2O5.

关键词： molybdophosphoric acid vanadia alumina oxidation benzyl alcohol