Abstract：
:3-(3-acetyl-4-hydroxyphenyl)-1,1-diethylurea (A-1354), is a synthetic intermediate of the beta-adrenergic blocker, celiprolol hydrochloride. A liquid chromatographic method has been developed and validated for the determination of bulk A-1354 and its potential impurities. High-low chromatography was used to improve the detectability of trace impurities. Enhanced chemical detectability was achieved by comparing the detector response of trace-impurity peaks from a stock sample solution (high-concentration) with the detector response for the A-1354 peak in a quantitatively diluted working sample solution (low-concentration). Chromatographic separation was achieved by gradient elution of A-1354 and its known impurities using an Ultrasphere C18 analytical column (5 microns, 250 x 4.6 mm i.d.). The gradient mobile phase components were methanol and 0.1% triethylammonium phosphate, pH = 4.0. The flow rate was 0.9 ml min-1 with UV absorbance detection at 236 nm. The method was determined to be specific, linear, precise and accurate for A-1354 and its known impurities. Known impurities of A-1354 are quantitated to 0.05% (w/w).
journal_name
J Pharm Biomed Analjournal_title
Journal of pharmaceutical and biomedical analysisauthors
Difeo TJ,Shuster JEdoi
10.1016/0731-7085(91)80008-wsubject
Has Abstractpub_date
1991-01-01 00:00:00pages
823-8issue
10-12eissn
0731-7085issn
1873-264Xpii
0731-7085(91)80008-Wjournal_volume
9pub_type
杂志文章abstract：:A fast headspace GC-MS method was developed and validated for the detection and quantification of residual solvents of all three ICH-classes in counterfeit tablets and capsules. The method was validated for 10 solvents, selected based on an initial screening of counterfeit medicinal products. The considered solvents w...
journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章
doi：10.1016/j.jpba.2012.05.022
更新日期：2012-11-01 00:00:00
abstract：:A simple HPLC-UV method was established for the determination of orientin in plasma and different tissues of rat (heart, liver, spleen, lung, kidney, brain, stomach and small intestine). The separation was achieved by HPLC on a C(18) column with a mobile phase composed of acetonitrile-0.1% acetic acid (20:80, v/v), UV...
journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章
doi：10.1016/j.jpba.2008.01.035
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journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章
doi：10.1016/s0731-7085(99)00157-0
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abstract：:Tramadol is a centrally acting analgesic drug used in veterinary and human clinical practice. Its metabolism has been largely characterized in human being but is still long to be comprehended in several animal species, especially in the dog. The aim of the present study was to develop and validate a new analytical pro...
journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章
doi：10.1016/j.jpba.2010.03.016
更新日期：2010-10-10 00:00:00
abstract：:Mepitiostane (2α,3α-epithio-17β-(1-methoxycyclopentyloxy)-5α-androstane), which is a prodrug of epitiostanol (2α,3α-epitio-5α-androstane-17β-ol), is an epitiosteroid having anti-estrogenic and weak androgenic anabolic activities. The World Anti-Doping Agency prohibits the misuse of mepitiostane by athletes. Detection ...
journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章
doi：10.1016/j.jpba.2015.07.016
更新日期：2015-11-10 00:00:00
abstract：:The controlled adsorptive accumulation of Zn(II)-terfenadine complex (1:1) onto a hanging mercury drop electrode (HMDE) provides the basis for determination of the antihistamine drug terfenadine by differential pulse cathodic adsorptive stripping voltammetry. The adsorbed Zn(II)-terfenadine complex (1:1) at the HMDE d...
journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章
doi：10.1016/s0731-7085(01)00491-5
更新日期：2001-11-01 00:00:00
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journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章
doi：10.1016/j.jpba.2017.03.038
更新日期：2017-07-15 00:00:00
abstract：:A new tadalafil analogue was detected and isolated from a dietary supplement, the structure was elucidated by means of nuclear magnetic resonance (NMR) and mass spectroscopy. The compound was determined to be diethylaminopretadalafil, which might be derived from a precursor in the synthesis of tadalafil. ...
journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章
doi：10.1016/j.jpba.2014.01.043
更新日期：2014-06-01 00:00:00
abstract：:Capillary electromigration techniques have become important tools for the analysis of pharmaceutical drugs. The present review updates on recent developments of the analysis of small molecule drugs, excipients and counter ions dating between January 2014 and May 2017. Capillary electrophoresis (CE) continues to be a v...
journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章,评审
doi：10.1016/j.jpba.2017.06.063
更新日期：2018-01-05 00:00:00
abstract：:The Mahuang-Xingren herb-pair (MX), the combination of Herba Ephedrae (Mahuang in Chinese) and Semen Armeniacae Amarum (Xingren in Chinese), is a classical combination used in traditional Chinese Medicine to treat asthma and bronchitis. A simple and reliable ultra-performance liquid chromatography-tandem mass spectrom...
journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章
doi：10.1016/j.jpba.2015.02.004
更新日期：2015-05-10 00:00:00
abstract：:Three extracts of Calendulae officinalis flos (Asteraceae): heptane, ethyl acetate and methanol were introduced to a human skin fibroblast (HSF) cells culture and a culture of human breast cancer cells (T47D), cell culture collection ECACC number 85102201. The ethyl acetate but not the heptane and methanol extracts in...
journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章
doi：10.1016/j.jpba.2004.12.034
更新日期：2005-06-15 00:00:00
abstract：:Two impurities showing structures 5 and 6 were isolated and characterised by means of NMR analysis, during the optimisation of a synthetic procedure to tazarotene. Impurity 5, i.e. ethyl 6-((4,4-dimethyl-4H-thiochromen-6-yl)ethynyl)nicotinate, was a by-product of the reduction of the intermediate sulfoxide 7 with PCl(...
journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章
doi：10.1016/j.jpba.2007.11.004
更新日期：2008-02-13 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：:Most drugs are excreted into breast milk to some extent and are bioavailable to the infant. The ability to predict the approximate amount of drug that might be present in milk from the drug structure would be very useful in the clinical setting. The aim of this research was to simplify and upgrade the previously devel...
journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章,评审
doi：10.1016/s0731-7085(02)00037-7
更新日期：2002-06-20 00:00:00
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journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章
doi：10.1016/s0731-7085(99)00087-4
更新日期：1999-09-01 00:00:00
abstract：:A differential pulse polarographic method is described for detection and trace determination of benzophenone (the main impurity) in phenytoin powder. The method depends upon the polarographic activity of benzophenone in Britton-Robinson buffer pH 5.6. The limit of detection was found to be 2.5 x 10(-6) microg ml(-1). ...
journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章
doi：10.1016/s0731-7085(01)00669-0
更新日期：2002-05-15 00:00:00
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 enantiom...
journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章
doi：10.1016/0731-7085(84)80043-6
更新日期：1984-01-01 00:00:00
abstract：:A selective, rapid and sensitive ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) method was developed for the quantitative determination of lovastatin in human plasma and its application in a pharmacokinetic study. With mycophenolate mofetil as internal standard, sample pretreatment invol...
journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章
doi：10.1016/j.jpba.2007.12.005
更新日期：2008-03-13 00:00:00
abstract：:A method of reducing disturbing peaks in LC-chromatograms is described. The technique, here called digital subtraction chromatography (DSCh), makes use of the new generation of integrating chromatographic data processors. These processors are able to store the LC-detector signal and then subtract one chromatogram from...
journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章
doi：10.1016/0731-7085(89)80069-x
更新日期：1989-01-01 00:00:00
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journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章
doi：10.1016/j.jpba.2019.112832
更新日期：2020-01-05 00:00:00
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journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章,评审
doi：10.1016/s0731-7085(01)00653-7
更新日期：2002-01-15 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：:Protandim is an over-the-counter herbal dietary supplement. The key components of Protandim, i.e., epigallocatechin-3-gallate (EGCG), silibinin (SIL), and curcumin (CUR) were simultaneously analyzed through a liquid chromatography-tandem mass spectrometric (LC-MS/MS) method in plasma and different tissues after admini...
journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章
doi：10.1016/j.jpba.2019.03.024
更新日期：2019-06-05 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：:LC-MS/MS is a promising analytical platform for the quantification of recombinant therapeutic proteins in biological fluids for pharmacokinetic (PK) studies. Herein, an absolute quantification method based on LC-MS/MS technique was developed to quantify endostar, which is modified from the recombinant human endostatin...
journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章
doi：10.1016/j.jpba.2012.07.017
更新日期：2012-11-01 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：:A methylene blue (MB) poly(vinyl chloride) membrane sensor based on MB-silicotungstate (SLT) ion association as electroactive material was described. The linear response covered the range 1 x 10(-3)-1 x 10(-6) mol x dm(-3) MB solution, with a slope 52.0+/-0.8 mV decade(-1) (pH range 3.0-10.0). The detection limit was ...
journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章
doi：10.1016/s0731-7085(98)00104-6
更新日期：1999-01-01 00:00:00
abstract：:Spectrophotometric procedures for the determination of two irriversible proton pump inhibitors, omeprazole (OMZ) and pantoprazole (PNZ) sodium have been developed, the procedures are based on the formation of 2:1 chelates of both drugs with different metal ions. Pantoprazole sodium is quantified by a stability-indicat...
journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章
doi：10.1016/s0731-7085(03)00233-4
更新日期：2003-10-15 00:00:00
abstract：:Aldehydes are very reactive carbonyl compounds that are widespread naturally. Aldehydes can be produced in vivo by oxidative reactions and are able to disturb biological functions through binding and modifying biomolecules. Thus, it is necessary to determine their levels in biological samples to estimate their possibl...
journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章,评审
doi：10.1016/j.jpba.2019.112782
更新日期：2019-10-25 00:00:00
abstract：:Serum metabolic profiling can identify the metabolites responsible for discrimination between doxycycline treated and untreated chronic obstructive pulmonary disease (COPD) and explain the possible effect of doxycycline in improving the disease conditions. 1H nuclear magnetic resonance (NMR)-based metabolomics was use...
journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章,随机对照试验
doi：10.1016/j.jpba.2016.09.034
更新日期：2017-01-05 00:00:00
