Abstract:
:A thermospray liquid chromatography/mass spectrometry (TSP-LC/MS) method is described for determination of the enantiomeric excess of alpha-amino acids and alpha-amino acid amides as their o-phthalaldehyde/N-acetyl-L-cysteine (OPA/NAC) derivatives. The source temperature is an important factor in optimizing the sensitivity of the TSP-LC/MS analysis, whereas the repeller voltage is of minor importance. On-column mass spectra were acquired for the OPA/NAC derivatives of several alpha-amino acids and alpha-amino acid amides. For the main fragment ions, mass spectra fragmentation pathways are proposed. The applicability of the method is demonstrated by means of the enantiomeric excess determination of valine in a sample from an enzymatic hydrolysis experiment. Using single ion monitoring, the detection limit of D-valine in the presence of excess L-valine is 10 pmol. The present TSP-LC/MS method is useful for validating the results obtained from LC/UV or LC/fluorescence methods for the enantiomeric excess determination of alpha-amino acids and alpha-amino acid amides.
journal_name
J Pharm Biomed Analjournal_title
Journal of pharmaceutical and biomedical analysisauthors
van Leuken RG,Duchateau AL,Kwakkenbos GTdoi
10.1016/0731-7085(95)01580-9subject
Has Abstractpub_date
1995-11-01 00:00:00pages
1459-64issue
12eissn
0731-7085issn
1873-264Xpii
0731708595015809journal_volume
13pub_type
杂志文章abstract::The water content of six different substances was determined by means of five different methods. The methods used were loss on drying, thermogravimetry (coupled with DSC), a new phosphorous-pentoxide method, direct Karl-Fischer titration and the Karl-Fischer oven. A combination of direct Karl-Fischer titration and the...
journal_title:Journal of pharmaceutical and biomedical analysis
pub_type: 杂志文章
doi:10.1016/j.jpba.2006.08.002
更新日期:2007-01-17 00:00:00
abstract::This paper proposes a method for the validation of chromatography systems in which many experiments to estimate SD or RSD are difficult or impossible to carry out because of time, cost, etc. HPLC systems with UV-Vis and fluorescence detectors and GC-MS system for bisphenol-A leached from hemodialyzers are taken as an ...
journal_title:Journal of pharmaceutical and biomedical analysis
pub_type: 杂志文章
doi:10.1016/s0731-7085(01)00698-7
更新日期:2002-05-15 00:00:00
abstract::Prostate cancer (CaP) is a leading cause of cancer deaths in men worldwide. The alarming statistics, the currently applied biomarkers are still not enough specific and selective. In addition, pathogenesis of CaP development is not totally understood. Therefore, in the present work, metabolomics study related to urinar...
journal_title:Journal of pharmaceutical and biomedical analysis
pub_type: 杂志文章
doi:10.1016/j.jpba.2014.12.026
更新日期:2015-01-01 00:00:00
abstract::Three different procedures for the labeling of hyaluronan (HA) with (111)In, (125)I and (14)C radionuclides were compared, and the kinetic stability of radiolabeled HA under different conditions (saline, artificial gastric juice and plasma) was established. Modification of HA structure with bifunctional chelating agen...
journal_title:Journal of pharmaceutical and biomedical analysis
pub_type: 杂志文章
doi:10.1016/j.jpba.2010.02.005
更新日期:2010-08-01 00:00:00
abstract::A systematic method in hydrophilic interaction chromatography (HILIC) was developed for the separation of four monophosphate nucleotides using design of experiment (DOE) approaches. Three HPLC parameters, the buffer concentration (ammonium acetate concentration), gradient time, and temperature, were evaluated within t...
journal_title:Journal of pharmaceutical and biomedical analysis
pub_type: 杂志文章
doi:10.1016/j.jpba.2018.05.014
更新日期:2018-09-05 00:00:00
abstract::6-O-Succinil-beta-cyclodextrin (CDsuc6) was synthesized with very good yield by one pot synthesis and characterized by NMR spectroscopy and ESI-MS. It was used as a chiral selector in capillary electrophoresis to resolve catecholamine racemates, namely norepinephrine, epinephrine, terbutaline and norphenilephrine. The...
journal_title:Journal of pharmaceutical and biomedical analysis
pub_type: 杂志文章
doi:10.1016/j.jpba.2004.08.023
更新日期:2005-04-29 00:00:00
abstract::The optimization of the HPLC procedures and the investigation of the predictive models are generally seen as distinct tasks although they could be both approached by very similar chemometric methods. In this work we used chemometric approaches to both optimize the separation of a non-steroidal anti-inflammatory drugs ...
journal_title:Journal of pharmaceutical and biomedical analysis
pub_type: 杂志文章
doi:10.1016/j.jpba.2009.08.001
更新日期:2010-01-05 00:00:00
abstract::Assessing the physical state of a low-dose active compound in a solid lipid or polymer matrix is analytically challenging, especially if the matrix exhibits some crystallinity. The aim of this study was first to compare the ability of current methods to detect the presence of a crystalline model compound in lipid matr...
journal_title:Journal of pharmaceutical and biomedical analysis
pub_type: 杂志文章
doi:10.1016/j.jpba.2015.06.033
更新日期:2015-11-10 00:00:00
abstract::The spectral, solubility and related physicochemical characteristics of the ovarian hormone are presented. A review of its crystal properties indicates that the common crystalline form of the steroid is the hemihydrate. ...
journal_title:Journal of pharmaceutical and biomedical analysis
pub_type: 杂志文章
doi:10.1016/0731-7085(87)80076-6
更新日期:1987-01-01 00:00:00
abstract::Obesity is one of the independent risk factors for several health problems, leading to metabolic perturbations and for which analytical approaches i.e., "metabolomics" is needed to monitor the underlying metabolic changes. In this study, obesity associated changes were assessed via serum metabolites analysis of obese ...
journal_title:Journal of pharmaceutical and biomedical analysis
pub_type: 杂志文章
doi:10.1016/j.jpba.2017.05.001
更新日期:2017-08-05 00:00:00
abstract::A new, rapid, simple and specific method to determine 5-chloro 8-hydroxyquinoline (5-HQ) and 5,7-dichloro 8-hydroxyquinoline (5,7-HQ) stability in swine feed was optimized and validated. A system consisting of an ACQUITY UPLC BEH C18 column (1.7 μm, 2.1 mm × 100 mm), a mobile phase of acetonitrile-0.1% o-phosphoric ac...
journal_title:Journal of pharmaceutical and biomedical analysis
pub_type: 杂志文章
doi:10.1016/j.jpba.2018.12.037
更新日期:2019-03-20 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::The anodic and cathodic behavior of nisoldipine, 3-isobutyl-5-methyl-1,4-dihydro-2,6-dimethyl-4-(2-nitrophenyl)pyridine-3 ,5-dicarboxylate, are reported. This drug belongs to the nitroaryl-1,4-dihydropyridine family, known as calcium channel antagonist and employed in therapeuticalls as peripheral and cerebral vasodil...
journal_title:Journal of pharmaceutical and biomedical analysis
pub_type: 杂志文章
doi:10.1016/s0731-7085(97)00122-2
更新日期:1998-01-01 00:00:00
abstract::A new HPLC method for the determination of paeoniflorin in rat serum with solid-phase extraction (SPE) for preconcentration is introduced. Paeoniflorin and an internal standard (pentoxifylline) were extracted from serum by means of SPE using cartridges with octadecyl chemically bound phase. The HPLC separation was the...
journal_title:Journal of pharmaceutical and biomedical analysis
pub_type: 杂志文章
doi:10.1016/s0731-7085(03)00294-2
更新日期:2003-10-15 00:00:00
abstract::In a multicentre study involving six laboratories, a microbiological assay was performed on three neomycin samples containing respectively, 0.12, 2.1 and 11% (m/m) of neomycin C, as well on a pure neomycin C sample. The potency was determined according to the European Pharmacopoeia method but using a neomycin B base s...
journal_title:Journal of pharmaceutical and biomedical analysis
pub_type: 杂志文章
doi:10.1016/s0731-7085(97)00247-1
更新日期:1998-08-01 00:00:00
abstract::In our previous work, a new monolithic coating based on vinylpyrrolidone-ethylene glycol dimethacrylate polymer was introduced for stir bar sorptive extraction. The formulation of the prepared vinylpyrrolidone-ethylene glycol dimethacrylate monolithic polymer was optimized and the satisfactory quality of prepared coat...
journal_title:Journal of pharmaceutical and biomedical analysis
pub_type: 杂志文章
doi:10.1016/j.jpba.2018.02.030
更新日期:2018-05-10 00:00:00
abstract::NMR spectroscopy has become an essential diagnostic tool for pharmaceutical preparations worldwide, with many runs performed annually on a routine basis. In this study multivariate analysis was performed on a big dataset of 990 NMR heparin spectra recorded over six years (2012-2017) in our laboratory. Several steps of...
journal_title:Journal of pharmaceutical and biomedical analysis
pub_type: 杂志文章
doi:10.1016/j.jpba.2019.05.024
更新日期:2019-09-05 00:00:00
abstract::The use of gradient supercritical fluid chromatography (SFC) for the impurity profiling of pharmaceutical products is not widely practiced. Historically, the limited advancement in SFC instrumentation and the lag in column development have resulted in marginal sensitivity, selectivity and reproducibility when compared...
journal_title:Journal of pharmaceutical and biomedical analysis
pub_type: 杂志文章
doi:10.1016/j.jpba.2012.05.025
更新日期:2012-11-01 00:00:00
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
更新日期:2003-08-08 00:00:00
abstract::CpG oligodeoxynucleotide 107 (CpG ODN107) could be used as a novel radiosensitizer for glioma. Herein, a novel and sensitive reversed-phase HPLC coupled with electrospray triple quadrupole mass spectrometry (LC-MS/MS) following a one-step C18 solid-phase extraction (SPE) for biological matrix removal was developed and...
journal_title:Journal of pharmaceutical and biomedical analysis
pub_type: 杂志文章
doi:10.1016/j.jpba.2012.06.022
更新日期:2012-11-01 00:00:00
abstract::The five active drug substances and two of the excipients present in Frenadol, a cold medication, were separated. The active drug components dextromethorphan HBr monohydrate, ascorbic acid, caffeine, paracetamol and chlorpheniramine maleate were quantitatively assayed by a mixed ion pair LC method. The excipients sepa...
journal_title:Journal of pharmaceutical and biomedical analysis
pub_type: 杂志文章
doi:10.1016/0731-7085(94)80014-6
更新日期:1994-01-01 00:00:00
abstract::A reversed-phase high-performance liquid chromatographic (RP-HPLC) separation method with UV spectrophotometric detection has been developed for the determination of major components in leaves and caulomas of Schisandra chinensis Baill. The flavonols (quercetin and kaempferol) and (E)-cinnamic acid were analysed after...
journal_title:Journal of pharmaceutical and biomedical analysis
pub_type: 杂志文章
doi:10.1016/s0731-7085(00)00539-2
更新日期:2001-03-01 00:00:00
abstract::JNK pathway activates c-Jun(s) which are responsible for cell apoptosis; as a result, inhibitors of JNK pathway have the potential to prevent dopaminergic neurons from death and decrease the loss of dopamine in substantia nigra pars compacta (SNpc). Recent in-vitro studies show that 1,9-pyrazoloanthrone (1,9-P) a pote...
journal_title:Journal of pharmaceutical and biomedical analysis
pub_type: 杂志文章
doi:10.1016/j.jpba.2015.12.004
更新日期:2016-02-20 00:00:00
abstract::As the global market for pharmaceuticals increases, the adverse consequences of different regulations and requirements are becoming more obvious. Discussions between the regulatory authorities for the European Community, United States and Japan under the International Conference on Harmonization (ICH) intended to remo...
journal_title:Journal of pharmaceutical and biomedical analysis
pub_type: 杂志文章
doi:10.1016/0731-7085(95)01578-7
更新日期:1995-12-01 00:00:00
abstract::Cocaine is one of the most worldwide used illicit drugs. We report a magnetic particles-based enzyme-linked immunoassay (mpEIA) method for the rapid and sensitive determination of cocaine (COC) in saliva, urine and serum samples. Under optimized conditions, the limits of detections were 0.09ngmL(-1) (urine), 0.15ngmL(...
journal_title:Journal of pharmaceutical and biomedical analysis
pub_type: 杂志文章
doi:10.1016/j.jpba.2016.03.004
更新日期:2016-06-05 00:00:00
abstract::Glycoconjugate vaccines based on the Vi capsular polysaccharide directed against Salmonella enterica serovar Typhi are licensed or in development against typhoid fever, an important cause of morbidity and mortality in developing countries. Quantification of free polysaccharide in conjugate vaccines is an important qua...
journal_title:Journal of pharmaceutical and biomedical analysis
pub_type: 杂志文章
doi:10.1016/j.jpba.2017.02.042
更新日期:2017-05-30 00:00:00
abstract::An analytical method was developed for the determination of the enantiomers of felodipine, a dihydropyridine-type calcium antagonist, in human blood plasma. Felodipine was extracted from plasma using toluene as extraction solvent. The enantiomers were separated on a cellulose tris(4-methyl benzoate) stationary phase (...
journal_title:Journal of pharmaceutical and biomedical analysis
pub_type: 杂志文章
doi:10.1016/s0731-7085(01)00582-9
更新日期:2002-01-15 00:00:00
abstract::In this work, a new solid phase spectrophotometric method in association with flow injection analysis for Vitamin B6 (pyridoxine) determination has been developed with direct measurement of light-absorption in C18 material. In the developed method, successive passage of the complex, previously formed in the flowing st...
journal_title:Journal of pharmaceutical and biomedical analysis
pub_type: 杂志文章
doi:10.1016/s0731-7085(03)00589-2
更新日期:2004-02-18 00:00:00
abstract::In this study, the development and validation of a high-performance liquid chromatography (HPLC) assay for determination of repaglinide concentration in human plasma for pharmacokinetic studies is described. Plasma samples containing repaglinide and an internal standard, indomethacin were extracted with ethylacetate a...
journal_title:Journal of pharmaceutical and biomedical analysis
pub_type: 杂志文章
doi:10.1016/j.jpba.2006.12.010
更新日期:2007-04-11 00:00:00
abstract::A novel light emitting diode (LED) array-based light induced fluorescence (LIF) sensor is presented as an analytical methodology for at-line cleaning verification within the pharmaceutical industry. This sensor differs from conventional LIF sensors through the ability to dynamically control both the LED excitation arr...
journal_title:Journal of pharmaceutical and biomedical analysis
pub_type: 杂志文章
doi:10.1016/j.jpba.2012.09.018
更新日期:2013-01-01 00:00:00