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Simultaneous enantioseparation and simulation studies of atenolol,metoprolol and propranolol on Chiralpak^■IG column using supercritical fluid chromatography

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Journal of Pharmaceutical Analysis 2021年第6期11卷 746-756页

作者： Pranav A.Pandya priyanka a.shah Pranav S.Shrivastav Department of Chemistry School of SciencesGujarat UniversityAhmedabad380009India

Enantioseparation of threeβ-blockers,i.e.,atenolol,metoprolol and propranolol,was studied on amylose tris(3-chloro-5-methylphenylcarbamate)immobilized chiral stationary phase using supercritical fluid chromatography(SFC).The effect of organic modifiers(methanol,isopropanol and their mixture),column temperature and back pressure on chiral separation ofβ-blockers was *** chromatographic separation with respect to resolution,retention,and analysis time was achieved using a mixture of CO_(2) and 0.1%isopropyl amine in isopropanol:methanol(50:50,V/V),in 75:25(V/V)*** the optimized conditions,the resolution factors(Rs)and separation factors(a)were greater than3.0 and 1.5,***,with increase in temperature(25-45℃)and pressure(100-150 bars)there was corresponding decrease in retention factors(k),a and ***,a reverse trend(a and Rs)was observed for atenolol with increase in *** thermodynamic data from van’t Hoff plots revealed that the enantioseparation was enthalpy driven for metoprolol and propranolol while entropy driven for *** understand the mechanism of chiral recognition and the elution behavior of the enantiomers,molecular docking studies were *** binding energies obtained from simulation studies were in good agreement with the elution order found experimentally and also with the free energy *** method was validated in the concentration range of 0.5-10μg/m L for all the *** limit of detection and limit of quantitation ranged from 0.126 to 0.137μg/m L and 0.376-0.414μg/m L,*** method was used successfully to analyze these drugs in pharmaceutical preparations.

关键词： Enantioseparation Supercritical fluid chromatography β-blockers Chiralpak^(■)IG column Molecular docking Binding energy

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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

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Fast and sensitive LC–MS/MS method for the simultaneous determination of lisinopril and hydrochlorothiazide in human plasma

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Journal of Pharmaceutical Analysis 2017年第3期7卷 163-169页

作者： Jaivik V.shah priyanka a.shah Priya V.shah Mallika Sanyal Pranav S.Shrivastav Department of Chemistry School of Sciences Gujarat University Department of Pharmacy M.S.University Department of Chemistry St.Xavier's College

A sensitive and rapid liquid chromatography-tandem mass spectrometry(LC–MS/MS) method has been developed for the simultaneous determination of lisinopril(LIS) and hydrochlorothiazide(HCTZ) in human plasma using their labeled internal standards(ISs). Sample pre-treatment involved solid phase extraction on Waters Oasis HLB cartridges using 100 μL of plasma, followed by liquid chromatography on Hypersil Gold C_(18)(50 mm×3.0 mm, 5 μm) column. The analytes were eluted within 2.0 min using acetonitrile-5.0 m M ammonium formate, p H 4.5(85:15, v/v) as the mobile phase. The analytes and ISs were analyzed in the negative ionization mode and quantified using multiple reaction monitoring. The method showed excellent linearity over the concentration range of 0.50–250.0 ng/m L for both the analytes. The intra-batch and inter-batch precision(% CV) was ≤5.26% and their extraction recoveries were in the range of 96.6%–103.1%. Matrix effect evaluated in terms of IS-normalized matrix factors ranged from 0.97 to 1.03 for both the analytes. The validated method was successfully applied to determine the plasma concentration of the drugs using 10 mg lisinopril and 12.5 mg hydrochlorothiazide fixed dose formulation in 18 healthy Indian volunteers.

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

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Application of an LC–MS/MS method for the analysis of amlodipine,valsartan and hydrochlorothiazide in polypill for a bioequivalence study

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Journal of Pharmaceutical Analysis 2017年第5期7卷 309-316页

作者： Jaivik V.shah Jignesh M.Parekh priyanka a.shah Priya V.shah Mallika Sanyal Pranav S.Shrivastav Department of Chemistry School of Sciences Gujarat University Department of Chemistry St.Xavier's College Department of Pharmacy M.S.University

A sensitive and selective method has been proposed for the simultaneous determination of amlodipine(AML),valsartan(VAL) and hydrochlorothiazide(HCTZ) in human plasma by liquid chromatography–tandem mass spectrometry(LC–MS/MS). The analytes and their deuterated analogs were quantitatively extracted from100 μL human plasma by solid phase extraction on Oasis HLB cartridges. The chromatographic separation of the analytes was achieved on a Chromolith RP18 e(100 mm × 4.6 mm) analytical column within 2.5 min. The resolution factor between AML and VAL, AML and HCTZ, and VAL and HCTZ was 2.9, 1.5 and 1.4, respectively,under isocratic conditions. The method was validated over a dynamic concentration range of 0.02–20.0 ng/m L for AML, 5.00–10,000 ng/m L for VAL and 0.20–200 ng/m L for HCTZ. Ion-suppression/enhancement effects were investigated by post-column infusion technique. The mean IS-normalized matrix factors for AML, VAL and HCTZ were 0.992, 0.994 and 0.998, respectively. The intra-batch and inter-batch precision(% CV) across quality control levels was ≤ 5.56% and the recovery was in the range of 93.4%–99.6% for all the analytes. The method was successfully applied to a bioequivalence study of 5 mg AML + 160 mg VAL + 12.5 mg HCTZ tablet formulation(test and reference) in 18 healthy Indian males under fasting. The mean log-transformed ratios of C max, AUC0–120 h and AUC0-inf and their 90% CIs were within 90.2%–102.1%. The assay reproducibility was demonstrated by reanalysis of 90 incurred samples.

关键词： Amlodipine Valsartan Hydrochlorothiazide LC–MS/MS Polypill Bioequivalence

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SPE-UPLC-MS/MS assay for determination of letrozole in human plasma and its application to bioequivalence study in healthy postmenopausal Indian women

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Journal of Pharmaceutical Analysis 2016年第4期6卷 276-281页

作者： Pravin G.Vanol Puran Singhal priyanka a.shah Jaivik V.shah Pranav S.Shrivastav Mallika Sanyal Chemistry Department St.Xavier's College Bioanalytical Department Alkem Laboratories Ltd. Department of Chemistry School of SciencesGujarat University

A rapid and sensitive ultra performance liquid chromatography-tandem mass spectrometry（UPLC-MS/MS） method is described for determination of letrozole in human *** solid phase extraction（SPE） of letrozole and letrozole-d4 on Orochem DVB-LP cartridges,chromatography was performed on Acquity UPLC BEH C_（18）（50 mm × 2.1 mm.1.7 μm） column using methanol-0.1%formic acid in water（85：15,v/v） as the mobile *** was carried out on a triple quadrupole mass spectrometer with an electrospray source,operated under positive ionization *** of letrozole and letrozole-d4 was done using multiple reaction monitoring（MRM） following the transitions at m/z286.2→217.0 and m/z 290.2→221.0,*** calibration plots were linear through the concentration range of 0.10-100 ng/mL（r^2 ≥ 0.9990） using 100 μL human *** extraction recovery of letrozole ranged from 94.3%to 96.2%and the intra-batch and inter-batch precision was ≤ 5.2%.The method was successfully applied to a bioequivalence study of letrozole after oral administration of2.5 mg tablet formulation to 16 healthy postmenopausal Indian *** assay reproducibility was also established through incurred sample reanalysis（ISR） of 74 subject samples.

关键词： Letrozole Letrozole-D4 UPLC-MS/MS Solid phase extraction Bioequivalence study

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Determination of lercanidipine in human plasma by an improved UPLC–MS/MS method for a bioequivalence study

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Journal of Pharmaceutical Analysis 2016年第2期6卷 87-94页

作者： Darshan V.Chaudhary Daxesh P.Patel priyanka a.shah Jaivik V.shah Mallika Sanyal Pranav S.Shrivastav Department of Chemistry School of Sciences Gujarat University Navrangpura Ahmedabad Gujarat 380009 India Laboratory of Metabolism Center for Cancer Research National Cancer Institute National Institutes of Health Building 37 Room 3106 Bethesda MD 20892 USA Department of Chemistry St. Xavier's College Navrangpura Ahmedabad Gujarat 380009 India

An improved and reliable ultra-performance liquid chromatography/tandem mass spectrometry （UPLC- MS/MS） method has been developed and validated for the determination of lercanidipine in human plasma. Plasma samples with lercanidipine-d3 as an internal standard （IS） were prepared by solid phase extraction on Phenomenex Strata-X cartridges using 100 μL of human plasma. Chromatographic analysis was performed on UPLC BEH C18 （50 mm × 2.1 mm, 1.7 μm） column under isocratic conditions. Linear calibration curves were obtained over a wide dynamic concentration range of 0.010-20.0 ng/mL. Matrix effect was assessed by post-column infusion, post-extraction spiking and standard-line slope methods. The mean extraction recovery was 〉 94% for the analyte and IS. Inter-batch and intra-hatch precision （% CV） across five quality controls was 〈 5.8%. Bioequivalence study was performed with 36 healthy sub- jects after oral administration of 10 mg of lercanidipine and the assay reproducibility was evaluated by reanalysis of 133 incurred samples.

关键词： Lercanidipine UPLC-MS/MS Bioequivalence Solid phase extraction Human plasma

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Selective and rapid determination of raltegravir in human plasma by liquid chromatography–tandem mass spectrometry in the negative ionization mode

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Journal of Pharmaceutical Analysis 2015年第2期5卷 101-109页

作者： Ajay Gupta Swati Guttikar priyanka a.shah Gajendra Solanki Pranav S.Shrivastav Mallika Sanyal Chemistry Department Kadi Sarva Vishwavidyalaya Sarva Vidyalaya Campus Sector 15/23 Bioanalytical Research Department Veeda Clinical Research Department of Chemistry School of Sciences Gujarat University Department of Chemistry St.Xavier’s College

A selective and rapid high-performance liquid chromatography–tandem mass spectrometry method was developed and validated for the quantification of raltegravir using raltegravir-d3 as an internal standard（IS）. The analyte and IS were extracted with methylene chloride and n-hexane solvent mixture from 100 mL human plasma. The chromatographic separation was achieved on a Chromolith RP-18 e endcapped C18（100 mm 4.6 mm） column in a run time of 2.0 min. Quantitation was performed in the negative ionization mode using the transitions of m/z 443.1-316.1 for raltegravir and m/z 446.1-319.0 for IS. The linearity of the method was established in the concentration range of 2.0–6000 ng/m *** mean extraction recovery for raltegravir and IS was 92.6% and 91.8%, respectively, and the IS-normalized matrix factors for raltegravir ranged from 0.992 to 0.999. The application of this method was demonstrated by a bioequivalence study on 18 healthy subjects.

关键词： Raltegravir LC–ESI–MS/MS Negative ionization mode Human plasma Bioequivalence study

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CD9 role in proliferation, rejuvenation, and therapeutic applications

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Genes & Diseases 2024年第3期11卷 95-97页

作者： Sai priyanka Kodam Neda Baghban Mujib Ullah Institutefor Immunityand Transplantation Stem Cell Biology and Regenerative MedicineSchool of MedicineMolecular Medicine Department of MedicineStanford UniversityPaloAltoCA94304USA

The CD9 gene,also known as the Tspan29 gene,codes for a protein called CD9,which is a member of the tetraspanin family of transmembrane proteins.^(1) The CD9 protein is involved in various cellular processes,including cell proliferation,differentiation,adhesion,and migration.^(1,2) CD9 has also been found to play a role in the regulation of stem cell proliferation and differentiation.

关键词： migration. therapeutic CD9

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Multi-omics:Powerful accelerator for uncovering plant specialized metabolic pathways:The case of leonurine

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Molecular Plant 2024年第1期17卷 13-15页

作者： priyanka Gupta Anuj Sharma Dinesh A.Nagegowda Molecular Plant Biology and Biotechnology Lab CSIR-Central Institute of Medicinal and Aromatic PlantsResearch CentreBengaluru 560065India Academy of Scientific and Innovative Research Ghaziabad 201002India

As sessile organisms,plants employ a unique adaptive strategy to survive harsh terrestrial environments and defend against or interact with coevolving animals and *** strategy involves expanding their metabolic systems,resulting in the production of plant specialized metabolites(PSMs)or natural ***,PSMs constitute a highly diverse group of compounds based on their common core structure,comprising terpenoids,phenylpropanoids,benzenoids,alkaloids and nitrogen-containing compounds,glucosinolates,indoles and sulfur-containing indole compounds,phenolics,and fatty acid derivatives(Garagounis et al.,2021).

关键词： expanding alkaloids sulfur

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Betulin protects against isoproterenol-induced myocardial injury by inhibiting NF-κB signaling and attenuating cardiac inflammation and oxidative stress in rats

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Asian Pacific Journal of Tropical Biomedicine 2024年第6期14卷 236-244页

作者： Hital shah Tejal Gandhi Gujarat Technological University AhmedabadGujarat 382424India Department of Pharmacology Anand Pharmacy CollegeAnandGujarat 388001India

Objective:To investigate the cardioprotective potential of betulin in isoproterenol(ISO)-induced myocardial injury in ***:Wistar rats were divided into five groups(n=10):normal,ISO,nebivolol 5 mg/kg,and betulin(20&40 mg/kg).Nebivolol and betulin were administered orally for 29 ***(85 mg/kg)was administered subcutaneously on day 27 and day 28 to induce myocardial *** day 29,blood was collected for determination of cardiac markers,and hemodynamic parameters were *** levels of oxidative stress markers and the gene expressions of apoptotic markers and inflammatory mediators were ***,2,3,5-triphenyltetrazolium chloride staining and histopathological analysis were also ***:Betulin reduced the size of myocardial infarction,decreased elevated levels of cardiac enzymes,and maintained hemodynamic *** also inhibited ISO-induced upregulation of Bax,caspase-3,NF-κB,and IL-6,enhanced endogenous antioxidant enzymes,and reduced lipid ***,pretreatment with betulin alleviated myocardial ischemic damage,as reflected by reduced myonecrosis,edema,and inflammatory ***:Betulin exhibits strong cardioprotective activity against ISO-induced myocardial injury by anti-inflammatory,anti-apoptotic,and antioxidant activities.

关键词： NF-κB Isoproterenol Betulin Myocardial injury Oxidative stress Inflammation Apoptosis

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