Optical purity determination and (1)H NMR spectral simplification with lanthanide shift reagents - V. Mephenytoin, 5-ethyl-3-methyl-5-phenyl-2,4-imidazolidinedione.

Abstract:

:The 60-MHz 1H NMR spectra of racemic mephenytoin, I, have been studied with the achiral shift reagent, tris(6,6,7,7,8,8,8-heptafluoro-2,2-dimethyl-3,5-octane-dionato) europium (III), II, and the chiral reagent, tris[3-(trifluoromethylhydroxy-methylene)-d-camphorato] europium (III), III. Moderate values of the enantiomeric shift differences, Delta, were clearly observed for the NCH3, NH, aryl and CCH3 resonances in CDCl3 solution at 28 degrees C with added III. The NCH3 and NH absorptions could be useful for direct assays of optical purity. Thus, for a 0.34 molal solution of I in CDCl3 with a molar ratio III:I of 0.138, the value of Delta for the NCH3 resonance was 3.1 Hz (0.052 ppm) with 32% valley resolution.

journal_name

J Pharm Biomed Anal

authors

Avolio J,Rothchild R

doi

10.1016/0731-7085(84)80043-6

subject

Has Abstract

pub_date

1984-01-01 00:00:00

pages

403-8

issue

3-4

eissn

0731-7085

issn

1873-264X

pii

0731-7085(84)80043-6

journal_volume

2

pub_type

杂志文章
  • A sensitive HPLC-UV method for quantifying vancomycin in biological matrices: Application to pharmacokinetic and biodistribution studies in rat plasma, skin and lymph nodes.

    abstract::Vancomycin (VCN) is an antibiotic used in the treatment of methicillin-resistant Staphylococcus aureus (MRSA)-derived infections. As it has a relatively narrow therapeutic window, it is imperative to develop a sensitive and reliable analytical method for drug monitoring and pharmacokinetic purposes. In the present stu...

    journal_title:Journal of pharmaceutical and biomedical analysis

    pub_type: 杂志文章

    doi:10.1016/j.jpba.2020.113429

    authors: Ramadon D,Courtenay AJ,Permana AD,Tekko IA,McAlister E,McCrudden MTC,McCarthy HO,Donnelly RF

    更新日期:2020-09-10 00:00:00

  • A micro-QuEChERS method coupled to GC-MS for the quantification of pesticides in specific maternal and fetal tissues.

    abstract::The aim of this study was to establish a new QuEChERS (quick, easy, cheap, effective, rugged and safe) method coupled to gas chromatography-mass spectrometry (GC-MS) detection for the evaluation of the pesticide biodistribution in specific maternal and fetal tissues. This method was validated for the quantification of...

    journal_title:Journal of pharmaceutical and biomedical analysis

    pub_type: 杂志文章

    doi:10.1016/j.jpba.2014.10.035

    authors: Brandhonneur N,De Sousa Mendes M,Lepvrier E,Flejou Esseiva E,Chevanne F,Le Corre P

    更新日期:2015-02-01 00:00:00

  • Bioanalysis of an oligonucleotide and its metabolites by liquid chromatography-tandem mass spectrometry.

    abstract::An ion-pair reversed phase liquid chromatography-tandem mass spectrometry (LC-MS/MS) method has been developed for the quantification of a phosphorothioate oligonucleotide (PS-OGN) PF-ODN and its metabolites 5'N-1/3'N-1, 5'N-2 and 5'N-3 in rat plasma. Plasma samples were prepared with an initial phenol/dichloromethane...

    journal_title:Journal of pharmaceutical and biomedical analysis

    pub_type: 杂志文章

    doi:10.1016/j.jpba.2010.01.040

    authors: Deng P,Chen X,Zhang G,Zhong D

    更新日期:2010-08-01 00:00:00

  • Simultaneous rapid quantification of ginsenoside Rg1 and its secondary glycoside Rh1 and aglycone protopanaxatriol in rat plasma by liquid chromatography-mass spectrometry after solid-phase extraction.

    abstract::Ginseng saponins isolated from ginseng, have been regarded as the principal constituents responsible for the biological activities. The aim of this study was to set up a liquid chromatography-mass spectrometry (LC-MS) method for simultaneously determine the concentration of Ginsenoside Rg1 and its secondary glycoside ...

    journal_title:Journal of pharmaceutical and biomedical analysis

    pub_type: 杂志文章

    doi:10.1016/j.jpba.2004.12.007

    authors: Sun J,Wang G,Haitang X,Hao L,Guoyu P,Tucker I

    更新日期:2005-06-01 00:00:00

  • Characterization of interaction and the effect of carbamazepine on the structure of human serum albumin.

    abstract::The binding of carbamazepine (CBZ) to human serum albumin (HSA) was investigated under simulative physiological conditions. In this study, intrinsic fluorescence of tryptophan-214 in HSA was monitored upon the addition of CBZ. Binding constant of CBZ-HSA was calculated by the remarkable static quenching effect of CBZ ...

    journal_title:Journal of pharmaceutical and biomedical analysis

    pub_type: 杂志文章

    doi:10.1016/j.jpba.2010.05.025

    authors: Kalanur SS,Seetharamappa J,Kalalbandi VK

    更新日期:2010-11-02 00:00:00

  • β-Cyclodextrin enhanced on-line organic solvent field-amplified sample stacking in capillary zone electrophoresis for analysis of ambroxol in human plasma, following liquid-liquid extraction in the 96-well format.

    abstract::A field-amplified sample stacking (FASS) and capillary zone electrophoresis (CZE) method is described for the quantification of ambroxol hydrochloride in human plasma, following liquid-liquid extraction in the 96-well format. The separation was carried out at 25 °C in a 31.2 cm × 75 μm fused-silica capillary with an a...

    journal_title:Journal of pharmaceutical and biomedical analysis

    pub_type: 临床试验,杂志文章

    doi:10.1016/j.jpba.2012.02.026

    authors: Li J,Bi Y,Wang L,Sun F,Chen Z,Xu G,Fan G

    更新日期:2012-07-01 00:00:00

  • The effect of anionic surfactant on poliovirus particles during capillary electrophoresis.

    abstract::Because of its essential role in SDS-PAGE, sodium dodecylsulphate (SDS) is generally associated with protein denaturation. However, for SDS-PAGE, proteins are linearized in the presence of SDS, following the exposure to high temperatures and reducing agents. In comparison, the conditions employed during a capillary el...

    journal_title:Journal of pharmaceutical and biomedical analysis

    pub_type: 杂志文章

    doi:10.1016/j.jpba.2012.07.033

    authors: Oita I,Halewyck H,Thys B,Rombaut B,Heyden YV

    更新日期:2012-12-01 00:00:00

  • Quantitation of tenofovir and emtricitabine in dried blood spots (DBS) with LC-MS/MS.

    abstract::A reversed-phase high performance liquid chromatographic (LC), tandem mass spectrometry (MS/MS) assay for the determination of tenofovir (TFV) and emtricitabine (FTC) in dried blood spots (DBS) from human whole blood was developed and validated. Whole blood samples were spotted, dried, and a 3mm punch was extracted wi...

    journal_title:Journal of pharmaceutical and biomedical analysis

    pub_type: 杂志文章

    doi:10.1016/j.jpba.2013.08.033

    authors: Zheng JH,Guida LA,Rower C,Castillo-Mancilla J,Meditz A,Klein B,Kerr BJ,Langness J,Bushman L,Kiser J,Anderson PL

    更新日期:2014-01-01 00:00:00

  • High-throughput assays on the chip based on metal nano-cluster resonance transducers.

    abstract::High throughput transducers using metal cluster resonance technology are based on surface-enhancement of metal cluster light absorption. These devices can be used for detection of biorecognitive binding, as well as structural changes of nucleic acids, proteins or any other polymer. The optical property for the analyti...

    journal_title:Journal of pharmaceutical and biomedical analysis

    pub_type: 杂志文章

    doi:10.1016/s0731-7085(00)00545-8

    authors: Mayer C,Stich N,Palkovits R,Bauer G,Pittner F,Schalkhammer T

    更新日期:2001-03-01 00:00:00

  • Optimization and validation of a CZE method for rufloxacin hydrochloride determination in coated tablets.

    abstract::A simple and rapid capillary electrophoresis method with UV detection was developed and validated for the determination of rufloxacin hydrochloride in coated tablets. An experimental design strategy (Doehlert design and desirability function) allowed the analytical parameters to be simultaneously optimized in order to...

    journal_title:Journal of pharmaceutical and biomedical analysis

    pub_type: 杂志文章

    doi:10.1016/s0731-7085(02)00054-7

    authors: Furlanetto S,Orlandini S,Porta EL,Coran S,Pinzauti S

    更新日期:2002-06-15 00:00:00

  • HPLC determination of sertraline in bulk drug, tablets and capsules using hydroxypropyl-beta-cyclodextrin as mobile phase additive.

    abstract::A sensitive and stereospecific high-performance liquid chromatography (HPLC) method for determination of sertraline in bulk drug, tablets and capsules was developed. Chromatography resolution of the sertraline enantiomeric forms and trans diastereoisomers was performed on Alltima C18 (250 mm x 4.6mm i.d., 5 microm) co...

    journal_title:Journal of pharmaceutical and biomedical analysis

    pub_type: 杂志文章

    doi:10.1016/j.japna.2003.08.013

    authors: Chen D,Jiang S,Chen Y,Hu Y

    更新日期:2004-01-27 00:00:00

  • Chemical profiling and quantification of monacolins and citrinin in red yeast rice commercial raw materials and dietary supplements using liquid chromatography-accurate QToF mass spectrometry: Chemometrics application.

    abstract::Red yeast rice (RYR) is prepared by fermenting rice with various strains of the yeast Monascus spp of the Aspergillaceae family. Depending on the Monascus strains and the fermentation conditions, the products may contain monacolins, pigments and citrinin as secondary metabolites. Authentic and commercial RYR samples w...

    journal_title:Journal of pharmaceutical and biomedical analysis

    pub_type: 杂志文章

    doi:10.1016/j.jpba.2014.07.039

    authors: Avula B,Cohen PA,Wang YH,Sagi S,Feng W,Wang M,Zweigenbaum J,Shuangcheng M,Khan IA

    更新日期:2014-11-01 00:00:00

  • Explore the effects of Huang-Lian-Jie-Du-Tang on Alzheimer's disease by UPLC-QTOF/MS-based plasma metabolomics study.

    abstract::Alzheimer's disease (AD) is a progressive neurodegenerative disease with neither definitive pathogenesis nor effective treatment method so far. Huang-Lian-Jie-Du-Tang (HLJDT) is a classic formula of traditional Chinese medicine (TCM) proven to have ameliorative effects on learning and memory deficits of dementia. Morr...

    journal_title:Journal of pharmaceutical and biomedical analysis

    pub_type: 杂志文章

    doi:10.1016/j.jpba.2017.12.053

    authors: Sun LM,Zhu BJ,Cao HT,Zhang XY,Zhang QC,Xin GZ,Pan LM,Liu LF,Zhu HX

    更新日期:2018-03-20 00:00:00

  • Serum levels of beta-trace protein and glomerular filtration rate--preliminary results.

    abstract::The aim of this study was to evaluate the relationship between serum levels of beta-trace protein (BTP), a low molecular weight (MW) protein, and glomerular filtration rate (GFR). GFR and serum levels of BTP, and for comparison creatinine (Creat), cystatin C (Cys) and beta 2-microglobulin (beta 2M), were measured in 6...

    journal_title:Journal of pharmaceutical and biomedical analysis

    pub_type: 杂志文章

    doi:10.1016/s0731-7085(03)00215-2

    authors: Donadio C,Lucchesi A,Ardini M,Donadio E,Giordani R

    更新日期:2003-08-08 00:00:00

  • Application of miniaturized near-infrared spectroscopy for quality control of extemporaneous orodispersible films.

    abstract::Extemporaneous oral preparations are routinely compounded in the pharmacy due to a lack of suitable formulations for special populations. Such small-scale pharmacy preparations also present an avenue for individualized pharmacotherapy. Orodispersible films (ODF) have increasingly been evaluated as a suitable dosage fo...

    journal_title:Journal of pharmaceutical and biomedical analysis

    pub_type: 杂志文章

    doi:10.1016/j.jpba.2017.11.068

    authors: Foo WC,Widjaja E,Khong YM,Gokhale R,Chan SY

    更新日期:2018-02-20 00:00:00

  • Study on degradation kinetics of 2-(2-hydroxypropanamido) benzoic acid in aqueous solutions and identification of its major degradation product by UHPLC/TOF-MS/MS.

    abstract::A RP-HPLC method was developed and validated for the degradation kinetic study of 2-(2-hydroxypropanamido) benzoic acid (HPABA), a promising anti-inflammatory drug, which would provide a basis for further studies on HPABA. The effects of pH, temperature, buffer concentration and ionic strength on the degradation kinet...

    journal_title:Journal of pharmaceutical and biomedical analysis

    pub_type: 杂志文章

    doi:10.1016/j.jpba.2015.04.012

    authors: Zhang Q,Guan J,Rong R,Zhao Y,Yu Z

    更新日期:2015-08-10 00:00:00

  • Rapid determination of amoxicillin in premixes by HPLC.

    abstract::A rapid analytical procedure for routine identification and quantification of amoxicillin in premixes by high performance liquid chromatography was developed and tested. The ground premix samples were extracted for 10 min using 100ml extraction mixture water-methanol (800:200, v/v). The extract was analyzed by reverse...

    journal_title:Journal of pharmaceutical and biomedical analysis

    pub_type: 杂志文章

    doi:10.1016/j.jpba.2004.10.010

    authors: Dousa M,Hosmanová R

    更新日期:2005-02-23 00:00:00

  • Screening and identification of neuroprotective compounds from Scrophularia buergeriana using cell extraction coupled with LC-MS.

    abstract::In the cell extraction_LC-MS method, when cells are incubated with natural product extracts, bioactive compounds selectively bind to extracellular or intracellular targets. The extracts and major compounds (phenylpropanoids and iridoid glycosides) of Scrophularia buergeriana Miquel have been reported to show neuroprot...

    journal_title:Journal of pharmaceutical and biomedical analysis

    pub_type: 杂志文章

    doi:10.1016/j.jpba.2017.10.018

    authors: Shin H,Medriano CA,Park B,Park YH,Lee KY

    更新日期:2018-01-30 00:00:00

  • (1)H-Nuclear magnetic resonance-based metabolic profiling of nonsteroidal anti-inflammatory drug-induced adverse effects in rats.

    abstract::Nonsteroidal anti-inflammatory drugs (NSAIDs), which are globally prescribed, exhibit mainly anti-inflammatory and analgesic effects but also can cause adverse effects including gastrointestinal erosions, ulceration, bleeding, and perforation. The purpose of this study was to investigate surrogate biomarkers associate...

    journal_title:Journal of pharmaceutical and biomedical analysis

    pub_type: 杂志文章

    doi:10.1016/j.jpba.2016.07.045

    authors: Um SY,Park JH,Chung MW,Choi KH,Lee HJ

    更新日期:2016-09-10 00:00:00

  • LC/MS/MS analysis of vesnarinone and its principal metabolites in plasma and urine.

    abstract::An LC/MS/MS assay was developed and successfully used to quantitate vesnarinone and its principal metabolites (OPC-8230, OPC-18136, and OPC-18137) in human plasma and urine. Samples were pre-treated with liquid-solid extraction followed by simultaneous monitoring of primary and daughter ions which were used for the id...

    journal_title:Journal of pharmaceutical and biomedical analysis

    pub_type: 杂志文章

    doi:10.1016/s0731-7085(98)00194-0

    authors: Tata PN,Schorno KS,Cowart TD,Bramer SL

    更新日期:1999-01-01 00:00:00

  • A simple LC-MS/MS method using HILIC chromatography for the determination of fosfomycin in plasma and urine: application to a pilot pharmacokinetic study in humans.

    abstract::A high performance liquid chromatography-tandem mass spectrometry (LC-MS/MS) method, using hydrophilic interaction liquid chromatography (HILIC) chromatography for the analysis of fosfomycin in human plasma and urine, has been developed and validated. The plasma method uses a simple protein precipitation using a low v...

    journal_title:Journal of pharmaceutical and biomedical analysis

    pub_type: 杂志文章

    doi:10.1016/j.jpba.2014.11.042

    authors: Parker SL,Lipman J,Roberts JA,Wallis SC

    更新日期:2015-02-01 00:00:00

  • Optimization and validation of a dissolution test for selegiline hydrochloride tablets by a novel rapid HPLC assay using a monolithic stationary phase.

    abstract::The present study reports the optimization and validation of a dissolution test for selegiline.HCl tablets using a new high-performance liquid chromatographic (HPLC) method. Rapid separation of the analyte from sample matrix was achieved in less than 60s using a Cromolith RP-18e monolithic column using UV detection at...

    journal_title:Journal of pharmaceutical and biomedical analysis

    pub_type: 杂志文章

    doi:10.1016/j.jpba.2007.11.039

    authors: Tzanavaras PD,Themelis DG,Zotou A,Stratis J,Karlberg B

    更新日期:2008-03-13 00:00:00

  • Rapid profiling of alkaloid analogues in Sinomenii Caulis by an integrated characterization strategy and quantitative analysis.

    abstract::Alkaloids, the principal constituents in the caulis of Sinomenium acutum, have gained an increasing interest over the past decades since they are widely employed as a clinical treatment for rheumatoid arthritis. In the present study, an integrated characterization strategy by combining mass defect filtering-based stru...

    journal_title:Journal of pharmaceutical and biomedical analysis

    pub_type: 杂志文章

    doi:10.1016/j.jpba.2019.06.011

    authors: Jiang ZM,Wang LJ,Pang HQ,Guo Y,Xiao PT,Chu C,Guo L,Liu EH

    更新日期:2019-09-10 00:00:00

  • Chemical profiling and quantitation of bioactive compounds in Platycladi Cacumen by UPLC-Q-TOF-MS/MS and UPLC-DAD.

    abstract::Platycladi Cacumen (PC) is a traditional Chinese medicine used for the treatment of hemorrhages, cough, asthma and hair loss. To get a better understanding of the chemical constituents in PC, ultra-high performance liquid chromatography coupled with electrospray ionization quadrupole time-of-flight tandem mass spectro...

    journal_title:Journal of pharmaceutical and biomedical analysis

    pub_type: 杂志文章

    doi:10.1016/j.jpba.2018.03.005

    authors: Zhuang B,Bi ZM,Wang ZY,Duan L,Lai CJ,Liu EH

    更新日期:2018-05-30 00:00:00

  • Apoptosis induction activity and molecular docking studies of survivin siRNA carried by Fe3O4-PEG-LAC-chitosan-PEI nanoparticles in MCF-7 human breast cancer cells.

    abstract::Delivery of small interfering RNAs (siRNAs) into cells still remains a challenge in gene delivery studies. Here, we investigated the ability of synthesized Fe3O4-PEG-LAC-chitosan-PEI nanoparticles for siRNA delivery of survivin as the model gene into cells. The cellular uptake of survivin siRNA carried by synthesized ...

    journal_title:Journal of pharmaceutical and biomedical analysis

    pub_type: 杂志文章

    doi:10.1016/j.jpba.2017.04.025

    authors: Arami S,Mahdavi M,Rashidi MR,Yekta R,Rahnamay M,Molavi L,Hejazi MS,Samadi N

    更新日期:2017-08-05 00:00:00

  • Analysis of a formulation containing lincomycin and spectinomycin by liquid chromatography with pulsed electrochemical detection.

    abstract::A reversed phase ion-pair liquid chromatographic method using a base deactivated column and pulsed electrochemical detection on a gold electrode is described. It allows the separation of a mixture of spectinomycin sulfate, lincomycin hydrochloride and their related substances. A step gradient was necessary to obtain a...

    journal_title:Journal of pharmaceutical and biomedical analysis

    pub_type: 杂志文章

    doi:10.1016/s0731-7085(02)00015-8

    authors: Szúnyog J,Adams E,Liekens K,Roets E,Hoogmartens J

    更新日期:2002-06-20 00:00:00

  • Capillary electrophoresis in analysis of veterinary drugs.

    abstract::Antibiotics are extensively applied in veterinary medicine for the treatment of various bacterial infections. Because of their use in food producing animals, the risk of occurrence of unwanted residues in edible products exists. To ensure human food safety, The European Union has defined maximum residue limits (MRLs) ...

    journal_title:Journal of pharmaceutical and biomedical analysis

    pub_type: 杂志文章

    doi:10.1016/s0731-7085(03)00195-x

    authors: Kowalski P,Oledzka I,Lamparczyk H

    更新日期:2003-08-08 00:00:00

  • A new high-performance liquid chromatography-tandem mass spectrometry method for the determination of sunitinib and N-desethyl sunitinib in human plasma: Light-induced isomerism overtaking towards therapeutic drug monitoring in clinical routine.

    abstract::Sunitinib is approved for advanced renal cell cancer, imatinib-resistant or -intolerant gastrointestinal stromal tumors and pancreatic neuroendocrine cancers. It is prescribed at a fixed dose but its plasma exposure shows large inter-individual variations. Taking into account the narrow therapeutic window and the posi...

    journal_title:Journal of pharmaceutical and biomedical analysis

    pub_type: 杂志文章

    doi:10.1016/j.jpba.2019.112949

    authors: Marangon E,Buzzo M,Posocco B,Gagno S,Zanchetta M,Iacuzzi V,Poetto AS,Guardascione M,Giodini L,Toffoli G

    更新日期:2020-02-05 00:00:00

  • Permeability and transport mechanism of trihexyphenidyl hydrochloride in Caco-2 cell monolayer model with a validated UPLC-MS/MS method.

    abstract::A rapid and sensitive ultra-high-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) method was applied to investigate the permeability characteristics and transport mechanism of trihexyphenidyl hydrochloride (TH) in D-hanks with the Caco-2 cells model. Analytes were separated using an Zorbax Exten...

    journal_title:Journal of pharmaceutical and biomedical analysis

    pub_type: 杂志文章

    doi:10.1016/j.jpba.2019.112924

    authors: Lu C,Fu K,Cao K,Wei J,Zhou J,Zhao D,Li N,Lu Y,Chen X,Zhang Y

    更新日期:2020-01-30 00:00:00

  • Relationship between immobilised artificial membrane chromatographic retention and the brain penetration of structurally diverse drugs.

    abstract::Retention factors were determined for a set of 26 drugs, for which brain/blood concentration data are available, using immobilised artificial membrane (IAM) chromatography. The compound set represented acidic, basic and neutral drugs from various structural classes. The relationship between IAM retention and lipophili...

    journal_title:Journal of pharmaceutical and biomedical analysis

    pub_type: 杂志文章,评审

    doi:10.1016/s0731-7085(96)01883-3

    authors: Salminen T,Pulli A,Taskinen J

    更新日期:1997-01-01 00:00:00