Abstract:
:The solution-phase hydrolysis kinetics of the Aprepitant (Emend) prodrug, Fosaprepitant Dimeglumine, were investigated using an HPLC chromatographic reactor approach. The term 'chromatographic reactor' refers to the use of an analytical-scale column as both a flow-through reactor and, simultaneously, as separation medium for the reactant(s) and product(s). Recently, we reported a novel mathematical treatment for the kinetic data obtained from chromatographic reactors, which we believe is superior to other treatments in terms of its accuracy, robustness and ease of implementation. In this work, we demonstrate that our treatment may be applied equally well to HPLC reactors, as previously we studied only GC reactors. It is found that the hydrolysis of Fosaprepitant Dimeglumine (FD) has an apparent activation energy of 107 kJ/mol when the reaction is investigated on-column, using the gradient elution conditions of the validated HPLC impurity profile method for this compound. For comparison, the activation energy determined for the same reaction occurring in a quiescent solution consisting of a fixed ratio of acetonitrile-0.1% v/v aqueous H3PO4 (50:50, v/v) is 91 kJ/mol, calculated using direct application of the Arrhenius equation. The data presented show that, when used as a screening tool, chromatographic reactors may be feasible for use in the pharmaceutical industry to quickly gauge the relative stabilities of various compounds with similar degradation pathways.
journal_name
J Pharm Biomed Analjournal_title
Journal of pharmaceutical and biomedical analysisauthors
Skrdla PJ,Abrahim A,Wu Ydoi
10.1016/j.jpba.2006.02.005subject
Has Abstractpub_date
2006-06-07 00:00:00pages
883-90issue
3eissn
0731-7085issn
1873-264Xpii
S0731-7085(06)00170-1journal_volume
41pub_type
杂志文章abstract::Chinese medicine formula (CMF) usually contains multiple herbs and its components are very complicated, which therapeutic effects are derived from the integrative activity of multiple components. Therefore, the screening of bioactive compounds in the formula is necessary, though it is very difficult, not only for eluc...
journal_title:Journal of pharmaceutical and biomedical analysis
pub_type: 杂志文章
doi:10.1016/j.jpba.2020.113331
更新日期:2020-07-15 00:00:00
abstract::Three impurities were detected in the LC/MS analysis of fluconazole bulk drug substance. Two of the impurities were unknowns having not been reported previously. Structural assignment of these impurities was carried out by LC/MS/MS using electrospray ionization source and an ion trap mass analyzer. Structural elucidat...
journal_title:Journal of pharmaceutical and biomedical analysis
pub_type: 杂志文章
doi:10.1016/j.jpba.2006.04.012
更新日期:2006-09-26 00:00:00
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
更新日期:2020-09-10 00:00:00
abstract::The new guidelines of the United States pharmacopeia (USP), European pharmacopeia (EP) and international conference on harmonization (ICH) regulating elemental impurities limits in pharmaceuticals signify the end of unspecific analysis of metals as outlined in USP 〈231〉. The new guidelines specify both daily doses and...
journal_title:Journal of pharmaceutical and biomedical analysis
pub_type: 杂志文章
doi:10.1016/j.jpba.2017.06.045
更新日期:2017-10-25 00:00:00
abstract::A simple, inexpensive and efficient sample preparation technique, three-phase hollow fiber liquid phase microextraction (HF-LPME), followed by high-performance liquid chromatography-ultra violet detection (HPLC-UV) was used for the analysis of warfarin in human plasma. Warfarin was extracted from 11.0 ml of aqueous so...
journal_title:Journal of pharmaceutical and biomedical analysis
pub_type: 杂志文章
doi:10.1016/j.jpba.2011.11.019
更新日期:2012-03-05 00:00:00
abstract::An analytical GC-MS method based on nonpolar fused silica capillary column was developed to analyze the lipophilic constituents, mainly alkamides, from the root extracts of Echinacea purpurea (L.) Moench. In particular, the proposed method was applied to evaluate the phytochemical impacts of cucumber mosaic cucumoviru...
journal_title:Journal of pharmaceutical and biomedical analysis
pub_type: 杂志文章
doi:10.1016/s0731-7085(02)00146-2
更新日期:2002-08-01 00:00:00
abstract::A reversed-phase high-performance liquid chromatography (RP-HPLC) method with UV-detection at room temperature has been developed for the analysis of insulin and its main degradation product, A21-desamido insulin. Octadecylsilica was used as stationary phase and a mixture of water and acetonitrile containing tetramety...
journal_title:Journal of pharmaceutical and biomedical analysis
pub_type: 杂志文章
doi:10.1016/s0731-7085(03)00336-4
更新日期:2003-09-15 00:00:00
abstract::A 785nm diode laser and probe with a 6mm spot size were used to obtain spectra of stationary powders and powders mixing at 50rpm in a high shear convective blender. Two methods of assessing the effect of particle characteristics on the Raman sampling depth for microcrystalline cellulose (Avicel), aspirin or sodium nit...
journal_title:Journal of pharmaceutical and biomedical analysis
pub_type: 杂志文章
doi:10.1016/j.jpba.2012.12.003
更新日期:2013-03-25 00:00:00
abstract::An integrated strategy based on characteristic fragment filter (CFF) supplemented by multivariate statistical analysis (MSA) for MSn chromatograms [(CFF)s MSA] was proposed for the large-scale detection of natural plant-derived ingredients in vivo. To prove the practicability of this [(CFF)s MSA] strategy, rhubarb was...
journal_title:Journal of pharmaceutical and biomedical analysis
pub_type: 杂志文章
doi:10.1016/j.jpba.2019.05.049
更新日期:2019-09-10 00:00:00
abstract::A new herbal health product marketed for enhancing erectile function, namely Power58 Platinum, was purchased over-the-counter in Hong Kong. The product was tested for adulteration with sildenafil, tadalafil, and vardenafil as well as their structurally modified analogues. A new analogue of vardenafil, in which the N-e...
journal_title:Journal of pharmaceutical and biomedical analysis
pub_type: 杂志文章
doi:10.1016/j.jpba.2007.12.004
更新日期:2008-03-13 00:00:00
abstract::We describe a simple method for evaluating the inhibition of collagen IV degradation by cathepsin B with a surface plasmon resonance (SPR) biosensor. The change in the SPR signal decreased with an increase in the concentration of cathepsin B inhibitors. The order of the inhibitory constant (Ki) obtained by the SPR met...
journal_title:Journal of pharmaceutical and biomedical analysis
pub_type: 杂志文章
doi:10.1016/j.jpba.2017.06.026
更新日期:2017-10-25 00:00:00
abstract::Unknown by-product associated with the synthesis of dapoxetine was isolated. The structure elucidation of this new compound using accurate mass data and NMR spectroscopy is presented herein. The unambiguous resonance assignment concluded to the formation of a tricyclic compound 4-phenyl-2H,3H,4H-naphtho[1,2-b]pyran, a...
journal_title:Journal of pharmaceutical and biomedical analysis
pub_type: 杂志文章
doi:10.1016/j.jpba.2014.04.002
更新日期:2014-08-05 00:00:00
abstract::Authentication of natural products is of major relevance in the context of manufactured drugs or herbal supplements since such active products generate a lucrative market. The analytical method to identify and quantify valuable natural products is critical for quality control and product assignment of herbal supplemen...
journal_title:Journal of pharmaceutical and biomedical analysis
pub_type: 杂志文章
doi:10.1016/j.jpba.2018.11.062
更新日期:2019-02-20 00:00:00
abstract::A high throughput method was developed and validated for the quantitative determination of LAG078, a lipid-lowering compound, in dog plasma obtained during toxicokinetic studies. The method was based on reverse phase liquid chromatographic separation of the analyte from plasma extract followed by turbo-ionspray (TIS) ...
journal_title:Journal of pharmaceutical and biomedical analysis
pub_type: 杂志文章
doi:10.1016/j.jpba.2004.02.020
更新日期:2004-06-29 00:00:00
abstract::A simple method for the simultaneous determination of five bioactive components (rutin, puerarin, daidzein esculin and esculetin) in traditional medicinal preparations by non-aqueous capillary electrophoresis with UV detection has been developed for the first time. A running buffer composed of 15% acetonitrile, 2.5% a...
journal_title:Journal of pharmaceutical and biomedical analysis
pub_type: 杂志文章
doi:10.1016/j.jpba.2005.03.018
更新日期:2005-09-01 00:00:00
abstract::Assessment of analytical variability is recognized as an important factor for the establishment of specifications. Estimation of the variance for an analytical procedure can be accomplished using a variety of approaches. The approach of variance component analysis was applied retrospectively, as well as prospectively,...
journal_title:Journal of pharmaceutical and biomedical analysis
pub_type: 杂志文章
doi:10.1016/s0731-7085(97)00266-5
更新日期:1998-03-01 00:00:00
abstract::A very sensitive and convenient nanobiosensor based on fluorescence resonance energy transfer (FRET) was developed for the detection of a 22-mer oligonucleotides sequence in Human Papillomavirus 18 virus (HPV18) gene. For this purpose, water-soluble CdTe quantum dots (QDs) were synthesized and, subsequently, amino-mod...
journal_title:Journal of pharmaceutical and biomedical analysis
pub_type: 杂志文章
doi:10.1016/j.jpba.2017.01.002
更新日期:2017-03-20 00:00:00
abstract::A solid phase fluorescence spectroscopic batch procedure for (acetyl) salicylic acid in drug formulations have been developed. The procedure is based on the sorption of salicylic acid (SA) on Sephadex DEAE A-25 anion exchanger gel (100 mg) by equilibration from an aqueous solution (10 or 25 ml) for 5 min; the equilibr...
journal_title:Journal of pharmaceutical and biomedical analysis
pub_type: 杂志文章
doi:10.1016/s0731-7085(02)00719-7
更新日期:2003-03-10 00:00:00
abstract::A bead injection spectroscopy-flow injection analysis (BIS-FIA) system for the spectrophotometric detection of promethazine and trifluoperazine is developed. The sensor is based in the oxidation of the phenothiazines by Fe(III) which is later determined by formation of the complex between Fe(II) and Ferrozine, [FeFz(3...
journal_title:Journal of pharmaceutical and biomedical analysis
pub_type: 杂志文章
doi:10.1016/j.jpba.2004.03.010
更新日期:2004-09-03 00:00:00
abstract::The current therapeutic strategies are based on the design of multifunctional drug candidates able to interact with various disease related targets. Drugs that have the ability to scavenge reactive oxygen species (ROS), beyond their main therapeutic action, may prevent the oxidative damage of biomolecules. Therefore, ...
journal_title:Journal of pharmaceutical and biomedical analysis
pub_type: 杂志文章
doi:10.1016/j.jpba.2015.06.006
更新日期:2015-10-10 00:00:00
abstract::A previously established method for the analysis of chlortetracycline by liquid chromatography using polystyrene-divinylbenzene stationary phases was examined in a multicentre study involving four laboratories and a total of 12 columns. Three chlortetracycline hydrochloride samples were analysed. The main component an...
journal_title:Journal of pharmaceutical and biomedical analysis
pub_type: 杂志文章
doi:10.1016/0731-7085(92)80029-m
更新日期:1992-02-01 00:00:00
abstract::Since culture-based methods are costly and time consuming, alternative methods are investigated for the quantification of probiotics in commercial products. In this work ATR- FTIR vibration spectroscopy was applied for the differentiation and quantification of live Lactobacillus (La 5) in mixed populations of live and...
journal_title:Journal of pharmaceutical and biomedical analysis
pub_type: 杂志文章
doi:10.1016/j.jpba.2018.03.009
更新日期:2018-05-30 00:00:00
abstract::A sensitive and rapid ultra performance liquid chromatography-tandem mass spectrometric (UPLC-MS/MS) method has been developed for the determination of 21-hydroxy deflazacort in human plasma using betamethasone as the internal standard (IS). After solid-phase extraction from 100 μL human plasma, the analyte and IS wer...
journal_title:Journal of pharmaceutical and biomedical analysis
pub_type: 杂志文章
doi:10.1016/j.jpba.2013.07.035
更新日期:2013-11-01 00:00:00
abstract::The possibility has been investigated of applying derivative analysis to a classical enzymatic-spectrophotometric method for lecithin determination for the purpose of developing an analytical direct method that does not require long pretreatment of the test sample even in the case of turbid samples. Several samples of...
journal_title:Journal of pharmaceutical and biomedical analysis
pub_type: 杂志文章
doi:10.1016/s0731-7085(02)00155-3
更新日期:2002-08-01 00:00:00
abstract::A specific and reliable liquid chromatography-electrospray ionization-tandem mass spectrometry method was developed for the simultaneous determination of tetrahydropalmatine (THP), tetrahydroberineper (THB), tetrahydrocoptisine (THC) and corydaline (CDL) in rat plasma using jatrorrhizine as internal standard. Plasma s...
journal_title:Journal of pharmaceutical and biomedical analysis
pub_type: 杂志文章
doi:10.1016/j.jpba.2012.09.001
更新日期:2013-01-01 00:00:00
abstract::Extensive assignments of resonances in the 600 MHz 1H-NMR spectra of cerebrospinal fluid are reported. These have been achieved by the measurement of a combination of two-dimensional experiments comprising homonuclear J-resolved, COSY45, and double-quantum filtered COSY (DQCOSY) spectra. By these means the previous to...
journal_title:Journal of pharmaceutical and biomedical analysis
pub_type: 杂志文章
doi:10.1016/0731-7085(93)80171-v
更新日期:1993-08-01 00:00:00
abstract::A rapid, sensitive and high throughput UHPLC-MS/MS method was established and validated to assay the concentration of 2-(2-hydroxypropanamido) benzoic acid (HPABA), a promising anti-inflammatory drug, in rat plasma. Plasma samples were processed by liquid-liquid extraction with ethyl acetate and separated on a Shim-pa...
journal_title:Journal of pharmaceutical and biomedical analysis
pub_type: 杂志文章
doi:10.1016/j.jpba.2014.02.008
更新日期:2014-07-01 00:00:00
abstract::MEGATON, a dietary supplement, was analyzed in order to detect PDE-5 inhibitors and their analogues. A new analogue of vardenafil could be detected by high-performance liquid chromatography (HPLC) analysis with a photodiode array detector (PDA). This compound was compared with sildenafil, tadalafil, and vardenafil as ...
journal_title:Journal of pharmaceutical and biomedical analysis
pub_type: 杂志文章
doi:10.1016/j.jpba.2010.09.022
更新日期:2011-02-20 00:00:00
abstract::IIIM-290, an orally bioavailable preclinical candidate is effective in human xenograft models of leukemia, colon and pancreatic cancer. The promising preclinical data of this lead candidate has shown its potential for clinical development. As a part of its preclinical development, impurity profiling of pilot scale bat...
journal_title:Journal of pharmaceutical and biomedical analysis
pub_type: 杂志文章
doi:10.1016/j.jpba.2018.12.027
更新日期:2019-03-20 00:00:00
abstract::A new agar-free bioautographic assay for xanthine oxidase (XO) inhibitors and superoxide scavengers on TLC layers was developed and validated. Compared to the first version of TLC bioautographic agar overlay method, our bioautographic assay greatly improved the sensitivity and quantification ability. The limit of dete...
journal_title:Journal of pharmaceutical and biomedical analysis
pub_type: 杂志文章
doi:10.1016/j.jpba.2017.11.077
更新日期:2018-02-20 00:00:00