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Synthesis and optical characterization of porous ZnO

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Journal of Advanced Ceramics 2013年第3期2卷 260-265页

作者： K.SOWRI BABU A.RAMACHAnDRA REDDY Ch.SUJATHA K.VEnUGOPAL REDDY a.n.mallika Department of Physics National Institute of Technology WarangalWarangal-506004Andhra PradeshIndia

In this paper,a simple and cheap method to prepare porous ZnO by using zinc nitrate,ethanol and triethanolamine(TEA)is *** as-prepared sample consisted of nano and micro *** sample was calcined at 300℃,400℃and 500℃with different heating *** 500℃,the nano pores disappeared but the sample maintained its micro *** emission scanning electron microscopy(FE-SEM)pictures confirmed that the size and growth of ZnO nanoparticles depended on the heating *** infrared(IR)absorption peak of Zn-O stretching vibration positioned at 457 cm^(-1)was split into two peaks centered at 518 cm^(-1)and 682 cm^(-1)with the change of *** results confirmed that Fourier transform infrared(FT-IR)spectrum was sensitive to variations in particle size,shape and *** photoluminescence(PL)spectrum of porous ZnO contained five emission peaks at 397 nm,437 nm,466 nm,492 nm and 527 *** intensity enhanced monotonously with increase of temperature and the change was rapid between temperatures of 300℃and 500℃.This was due to the elimination of organic species and improvement in the crystallanity of the sample at 500℃.

关键词： semiconductors porous ZnO optical properties

Determination of asenapine in presence of its inactive metabolites in human plasma by LC-MS/MS

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Journal of Pharmaceutical Analysis 2018年第5期8卷 341-347页

作者： nirav R Patel mallika Sanyal naveen Sharma Dinesh S.Patel Pranav S.Shrivastav Bhavin n.Patel Bioanalytical Laboratory Uiantha Research India Ltd.BodakdevAhmedabad 380054GujaratIndia Kadi Sarva Viswavidyalaya Sector-15Ghandhinagar 382715GujaratIndia Department of Chemistry St.Xavier's CollegeNavrangpuraAhmedabad 380009GujaratIndia Department of Chemistry School of SciencesGujarat UniversityNavrangpuraAhmedabad 380009GujaratIndia

A highly selective and sensitive liquid chromatography-tandem mass spectrometry （LC-MS/MS） assay has been described for the determination of asenapine （ASE） in presence of its inactive metabolites n-desmethyl asenapine （DMA） and asenapine-n-glucuronide （ASG）. ASE, and ASE 13C-d3, used as internal standard （IS）, were extracted from 300 μL human plasma by a simple and precise liquid-liquid extraction procedure using methyl tert-butyl ether. Baseline separation of ASE from its inactive metabolites was achieved on Chromolith Performance RPse （100 mm ×4.6 mm） column using acetonitrile- 5.0 mM ammonium acetate-10% formic acid （90：10：0.1, v/v/v） within 4.5 min. Quantitation of ASE was done on a triple quadrupole mass spectrometer equipped with electrospray ionization in the positive mode. The protonated precursor to product ion transitions monitored for ASE and ASE 13C-d3 were m/z 286.1 → 166.0 and m/z 290.0 → 166.1, respectively. The limit of detection （LOD） and limit of quantitation （LOQ） of the method were 0.0025 ng/mL and 0.050 ng/mL respectively in a linear concentration range of 0.050-20.0 ng/mL for ASE. The intra-batch and inter-batch precision （% CV） and mean relative recovery across quality control levels were 〈 5.8% and 87.3%, respectively. Matrix effect, evaluated as IS-normalized matrix factor, ranged from 1.03 to 1.05. The stability of ASE under different storage conditions was ascertained in presence of the metabolites. The developed method is much simpler, matrix free, rapid and economical compared to the existing methods. The method was suc- cessfully used for a bioequivalence study of asenapine in healthy Indian subjects for the first time.

关键词： Asenapine Asenapine 13C-d3 Metabolites LC-MS/MS Bioequivalence study Human plasma

Geochemistry of eclogites of the Tso Morari complex, Ladakh, nW Himalayas:Insights into trace element behavior during subduction and exhumation

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Geoscience Frontiers 2019年第3期10卷 811-826页

作者： mallika K.Jonnalagadda nitin R.Karmalkar Raymond A.Duraiswami Department of Geology Savitribai Phule Pune University

Whole rock major and trace element compositions of seven eclogites from the Tso Morari ultra-high pressure(UHP) complex, Ladakh were determined with the aim of constraining the protolith origins of the subducted crust. The eclogites have major element compositions corresponding to sub-alkaline basalts. Trace element characteristics of the samples show enrichment in LILE's over HFSEs(Rb, Th, K except Ba) with LREE enrichments((La/Lu)n = 1.28-5.96). Absence of Eu anomaly on the Primitive Mantle normalized diagram suggests the absence of plagioclase fractionation. Positive correlation between Mg# with ni and Cr suggests olivine fractionation of mantle melts. narrow range of(La/Yb)n(2.1-9.4) and Ce/Yb(6.2-16.2) along with Ti/Y(435-735) ratios calculated for the Tso Morari samples is consistent with generation of melts by partial melting of a garnet free mantle source within the spinel peridotite field. Ternary diagrams(viz. Ti-Zr-Y and nb-Zr-Y) using immobile and incompatible elements show that the samples range from depleted to enriched and span from within plate basalts(WPB)to enriched MORB(E-MORB) indicating that the eclogite protoliths originated from basaltic *** Mantle normalized multi element plots showing significant Th and LREE enrichment marked by negative nb anomalies are characteristic of continental flood basalts. Positive Pb, negative nb, high Th/Ta, a narrow range of nb/La and the observed wide variation for Ti/Y indicate that the Tso Morari samples have undergone some level of crustal contamination. Observed geochemical characteristics of the Tso Morari samples indicate tholeiitic compositions originated from enriched MORB(E-MORB) type magmas which underwent a limited magmatic evolution through the process of fractional crystallization and probably more by crustal contamination. Observed geochemical similarities(viz. Zr, nb, La/Yb, La/Gd,La/nb, Th/Ta ratios and REE) between Tso Morari eclogites and the Group I Panjal Traps make the trap basa

关键词： Trace elements UHP metamorphism Protolith Eclogites Tso Morari Ladakh

Highly sensitive LC–MS/MS method to estimate doxepin and its metabolite nordoxepin in human plasma for a bioequivalence study

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Journal of Pharmaceutical Analysis 2018年第6期8卷 378-385页

作者： nirav P.Patel mallika Sanyal naveen Sharma Dinesh S.Patel Pranav S.Shrivastav Bhavin n.Patel Bio-Analytical Laboratory Cliantha Research India Ltd.BodakdevAhmedabad 380054GujaratIndia Kadi Sarva Viswavidyalaya Sector-15Ghandhinagar 382715GujaratIndia Department of Chemistry St.Xavier's CollegeNavrangpuraAhmedabad 380009GujaratIndia Department of Chemistry School of SciencesGujarat UniversityNavrangpuraAhmedabad 380009GujaratIndia

A selective, sensitive and rugged liquid chromatography–tandem mass spectrometry(LC–MS/MS) assay has been developed for the simultaneous determination of doxepin(Dox) and its pharmacologically active metabolite, nordoxepin(nDox) in human plasma. The analytes and their internal standards(IS)were extracted from 500 m L of human plasma by liquid-liquid extraction using methyl tert-butyl *** separation was achieved on Hypurity C8 column(100 mm ? 4.6 mm, 5 mm) using a mixture of acetonitrile-methanol(95:5, v/v) and 2.0 mM ammonium formate in 93:7(v/v) ratio. Detection was accomplished by tandem mass spectrometry in the positive ionization and multiple reaction monitoring acquisition mode. The protonated precursor to product ion transitions studied for Dox, nDox,and their corresponding ISs, propranolol and desipramine, were m/z 280.1-107.0, 266.0-107.0,260.1-116.1 and 267.1-72.1, respectively. A linear dynamic range of 15.0–3900 pg/mL for Dox and 5.00–1300 pg/mL for nDox was established with mean correlation coefficient(r2) of 0.9991 and 0.9993, respectively. The extraction recovery ranged from 86.6%–90.4% and 88.0%–99.1% for Dox and nDox, respectively. The intra-batch and inter-batch precision(% CV) across quality control levels was r 8.3% for both the analytes. Stability evaluated under different storage conditions showed no evidence of degradation and the % change in stability samples compared to nominal concentration ranged from 4.7% to12.3%. The method was successfully applied to a bioequivalence study of 6 mg doxepin hydrochloride orally disintegrating tablet in 41 healthy Indian subjects under fasting and fed conditions.

关键词： Doxepin nordoxepin LC–MS/MS Liquid-liquid extraction Human plasma Bioequivalence study

Simultaneous quantification of amiloride and hydrochlorothiazide in human plasma by liquid chromatography–tandem mass spectrometry

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Journal of Pharmaceutical Analysis 2017年第5期7卷 288-296页

作者： Jaivik V.Shah Priyanka A.Shah mallika Sanyal Pranav S.Shrivastav Department of Chemistry School of Sciences Gujarat University Department of Chemistry St.Xavier's College

A selective, sensitive and precise assay based on solid phase extraction and liquid chromatography–tandem mass spectrometry(LC–MS/MS) was developed for the simultaneous determination of amiloride(AMI) and hydrochlorothiazide(HCTZ) in human plasma. Sample clean-up with 250 μL of plasma was done on Phenomenex Strata^(?)-X extraction cartridges using their labeled internal standards(AMI-15 n3 and HCTZ-13 C,d2). Chromatography was performed on Hypersil Gold C18(50 mm×3.0 mm, 5 μm) column using acetonitrile with 4.0 m M ammonium formate(p H 4.0, adjusted with 0.1% formic acid)(80:20, v/v) as the mobile phase. Detection was carried out on a triple quadrupole API 5500 mass spectrometer utilizing an electrospray ionization interface and operating in the positive ionization mode for AMI and negative ionization mode for HCTZ. Multiple reaction monitoring was used following the transitions at m/z 230.6/116.0, m/z233.6/116.0, m/z 296.0/204.9 and m/z 299.0/205.9 for AMI, AMI-15 n3, HCTZ and HCTZ-13 C,d2,respectively. Calibration curves were linear(r2≥0.9997) over the concentration range of 0.050–50.0 and0.50–500 ng/m L for AMI and HCTZ, respectively, with acceptable accuracy and precision. The signal-to-noise ratio at the limit of quantitation was ≥14 for both the analytes. The mean recovery of AMI and HCTZ from plasma was 89.0% and 98.7%, respectively. The IS-normalized matrix factors determined for matrix effect ranged from 0.971 to 1.024 for both the analytes. The validated LC–MS/MS method was successfully applied to a bioequivalence study using 5 mg AMI and 50 mg HCTZ fixed dose tablet formulation in 18 healthy Indian volunteers with good reproducibility.

关键词： Amiloride Hydrochlorothiazide LC–MS/MS Solid phase extraction Human plasma

Simultaneous analysis of allopurinol and oxypurinol using a validated liquid chromatography–tandem mass spectrometry method in human plasma

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Journal of Pharmaceutical Analysis 2017年第1期7卷 56-62页

作者： Dhiraj M. Rathod Keyur R. Patel Hiren n. Mistri Arvind G. Jangid Pranav S. Shrivastav mallika Sanyal Department of Chemistry Kadi Sarva Vishwavidyalaya Gandhinagar Ahmedabad 382015 India Bioanalytical Research Department Accutest Research Lab Bodakdev Ahmedabad 380059 India Department of Chemistry School of Sciences Gujarat University Ahmedabad 380009 India Department of Chemistry St. Xavier's College Navrangpura Ahmedabad 380009 India

The present study describes a simple, reliable and reproducible liquid chromatography–tandem mass spectrometry method(LC–MS/MS) for the simultaneous determination of allopurinol and its active metabolite,oxypurinol in human plasma for a pharmacokinetic/bioequivalence study. After protein precipitation(PPT) of100 μL plasma sample with 1.0% formic acid in acetonitrile, the recovery of the analytes and allopurinol-d2 as an internal standard ranged from 85.36% to 91.20%. The analytes were separated on Hypersil Gold(150 mm×4.6 mm, 5 μm) column using 0.1% formic acid-acetonitrile(98:2, v/v) as the mobile *** was done using electrospray ionization in the positive mode. The calibration concentration range was established from 60.0 to 6000 ng/m L for allopurinol and 80.0–8000 ng/m L for oxypurinol. Matrix effect in human plasma, expressed as IS-normalized matrix factors ranged from 1.003 to 1.030 for both the analytes. The developed method was found suitable for a clinical study with 300 mg allopurinol tablet formulation in healthy subjects.

关键词： Allopurinol Oxypurinol Liquid chromatography–tandem mass spectrometry Bioequivalence study

An improved LC–MS/MS method for the quantification of alverine and para hydroxy alverine in human plasma for a bioequivalence study

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Journal of Pharmaceutical Analysis 2017年第2期7卷 95-102页

作者： Dhiraj M.Rathod Keyur R.Patel Hiren n.Mistri Arvind G.Jangid Pranav S.Shrivastav mallika Sanyal Department of Chemistry Kadi Sarva VishwavidyalayaGandhinagarAhmedabad-382015India Bioanalytical Research Department Accutest Research LabBodakdevAhmedabad-380059India Department of Chemistry School of SciencesGujarat UniversityAhmedabad-380009India Department of Chemistry St.Xavier's CollegeNavrangpuraAhmedabad-380009India

A highly sensitive and selective high performance liquid chromatography–tandem mass spectrometry method was developed and validated for the quantification of alverine（ALV） and its active metabolite, para hydroxy alverine（PHA）, in human plasma. For sample preparation, solid phase extraction of analytes was performed on Phenomenex Strata-X cartridges using alverine-d5 as the internal standard. The analytes were separated on Symmetry Shield RP18（150 mm×3.9 mm, 5 μm） column with a mobile phase consisting of acetonitrile and10 mM ammonium formate（65：35, v/v）. Detection and quantitation was done by electrospray ionization mass spectrometry in the positive mode using multiple reaction monitoring. The assay method was fully validated over the concentration range of 15.0–15,000 pg/mL for ALV and 30.0–15,000 pg/mL for PHA. The intra-day and inter-day accuracy and precision（% CV） ranged from 94.00% to 96.00% and 0.48% to 4.15% for both the analytes. The mean recovery obtained for ALV and PHA was 80.59% and 81.26%, respectively. Matrix effect,expressed as IS-normalized matrix factor ranged from 0.982 to 1.009 for both the analytes. The application of the method was demonstrated for the specific analysis of ALV and PHA for a bioequivalence study in 52 healthy subjects using 120 mg ALV capsules. The assay reproducibility was also verified by reanalysis of 175 incurred subject samples.

关键词： Alverine Para hydroxy alverine Liquid chromatography–tandem mass spectrometry Bioequivalence study Human plasma

Liquid chromatography-tandem mass spectrometry method for simultaneous determination of albendazole and albendazole sulfoxide in human plasma for bioequivalence studies

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Journal of Pharmaceutical Analysis 2016年第4期6卷 226-234页

作者： Dhiraj M.Rathod Keyur R.Patel Hiren n.Mistri Arvind G.Jangid Pranav S.Shrivastav mallika Sanyal Department of Chemistry Kadi Sarva Vishwavidyalaya Bioanalytical Research Department Accutest Research Lab Department of Chemistry School of SciencesGujarat University Department of Chemistry St.Xavier's College

An improved high performance liquid chromatography-tandem mass spectrometry（LC-MS/MS） method has been developed for sensitive and rapid determination of albendazole（ABZ） and its active metabolite,albendazole sulfoxide（ABZSO）,in the positive ionization *** method utilized solid phase extraction（SPE） for sample preparation of the analytes and their deuterated internal standards（ISs） from100 μL human *** chromatography was carried out on Hypurity C_（18） column using acetonitrile-2.0 mM ammonium acetate,pH 5.0（80：20,v/v） as the mobile *** assay exhibited a linear response over the concentration range of 0.200-50.0 ng/mL for ABZ and 3.00-600 ng/mL for *** recoveries of the analytes and ISs ranged from 86.03%-89.66%and 89.85%-98.94%,*** effect,expressed as IS-normalized matrix factors,ranged from 0.985 to 1.042 for the both *** method was successfully applied for two separate studies in healthy subjects using single dose of 400 mg conventional tablets and 400 mg chewable ABZ tablets,respectively.

关键词： Albendazole Albendazole sulfoxide LC-MS/MS Solid phase extraction Bioequivalence study

Geodynamic evolution of the Tethyan lithosphere as recorded in the Spontang Ophiolite,South Ladakh ophiolites(nW Himalaya,India)

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Geoscience Frontiers 2022年第1期13卷 326-349页

作者： mallika K.Jonnalagadda Mathieu Benoit Shivani Harshe Romain Tilhac Raymond A.Duraiswami Michel Grégoire nitin R.Karmalkar Interdisciplinary School of Science Savitribai Phule Pune UniversityPune 411007India Department of Geology Savitribai Phule Pune UniversityPune 411007India Géosciences Environnement Toulouse CNRS-CNES-IRD-UniversitéPaul SabatierObservatoire Midi Pyrénées31400 ToulouseFrance Instituto Andaluz de Ciencias de la Tierra(IACT) CSIC–Universidad de Granada18100 ArmillaGranadaSpain Vice-Chancellor’s Office Savitribai Phule Pune UniversityPune 411007India

The Spontang Ophiolite complex represents the most complete ophiolite sequence amongst the South Ladakh ophiolites and comprises mantle rocks(depleted harzburgites,dunites and minor lherzolites)as well as crustal rocks(basalt,isotropic gabbros,layered gabbros etc.).In the present study,detailed geochemistry(whole rock as well as mineral chemistry)and Sr-nd isotopic analyses of thirty-six ultramaficmafic samples have been attempted to constraint the evolution and petrogenetic history of the Tethyan oceanic ***,trace-element and REE patterns of the peridotites and their minerals indicate that the lherzolites experienced lower degrees of partial melting resembling abyssal peridotites(at higher temperatures,TREE=$1216℃)than the harzburgites(6%–8%versus 15%–17%).Elevated end(t)and variable^(87) Sr/^(86) Sr(t)ratios along with REE patterns suggest that the Spontang mafic rocks display n-MORB affinity with negligible participation of oceanic sediments in their genesis are originated from a depleted upper mantle with little contribution from subduction-related ***-type neotethyan oceanic crust is associated with the earliest phase of subduction(of older Jurassic age)through which a younger intra-oceanic island arc(Spong arc)subsequently *** REE display typical U-shaped patterns,suggesting that these rocks have been metasomatized by LREE-enriched *** the other side,mafic rocks are characterized by heterogeneous(nb/La)PMand(Hf/Sm)PMand relatively homogeneous end(t),indicating interaction of subduction-related melts with the upper mantle during the initiation of subduction,in Early Cretaceous times.

关键词： Peridotites Mafic rocks Partial melting Metasomatism Ladakh