Abstract：
:A robust gradient high performance liquid chromatographic (HPLC) procedure is described for the simultaneous determination of melphalan content and related impurities in melphalan drug substance. The sample solution is prepared in methanol and injected. A linear gradient from 5 to 60% acetonitrile in water containing 0.05% v/v acetic acid, 0.01% v/v triethylamine, and 0.05% w/v ammonium acetate is applied over 20 min. The chromatographic conditions are capable of separating and quantifying all impurities found in routine production batches of melphalan at above 0.1% area/area. The method has been fully validated and is linear over the column loading range of 0-3 microg of melphalan. All related impurities occurring in routine batches at above 0.1% area/area have been identified, and structures assigned. The method has been applied to melphalan samples stored under stressed conditions, and shown to be stability-indicating.
journal_name
J Pharm Biomed Analjournal_title
Journal of pharmaceutical and biomedical analysisauthors
Brightman K,Finlay G,Jarvis I,Knowlton T,Manktelow CTdoi
10.1016/s0731-7085(99)00011-4subject
Has Abstractpub_date
1999-07-01 00:00:00pages
439-47issue
3eissn
0731-7085issn
1873-264Xpii
S0731-7085(99)00011-4journal_volume
20pub_type
杂志文章abstract：:223 lip articles (representing 55 brands) were purchased in 15 European Union Member States and analysed for lead content. Various lip products (lipsticks and lip glosses), shades (red, brown, purple and pink) and price ranges (3 categories) were investigated. The analytical method employed a microwave-assisted acid d...
journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章
doi：10.1016/j.jpba.2012.11.047
更新日期：2013-03-25 00:00:00
abstract：:Rapamycin or sirolimus is a carboxylic lactone-lactam macrolide with a potent immunosuppressive activity. It can be successfully used to impregnate stents inserted in coronary arteries during surgical applications, preventing fatal infection and rejection adverse effect. The chemical stability of rapamycin in several ...
journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章
doi：10.1016/j.jpba.2006.02.009
更新日期：2006-06-07 00:00:00
abstract：:In search for new enantioselectivity profiles, the N-decyl-S-trityl-(R)-cysteine [C10-(R)-STC] was synthesized through a one-step procedure and then hydrophobically adsorbed onto an octadecylsilica surface to generate a stable chiral stationary phase for ligand-exchange chromatography (CLEC-CSP) applications. The CLEC...
journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章
doi：10.1016/j.jpba.2017.02.009
更新日期：2017-09-10 00:00:00
abstract：:CDRI compound 81/470 is a new broad spectrum anthelmintic agent and is being developed for veterinary use. HPLC assay method for 81/470 in cow milk was developed and validated. The sample preparation consisted of protein precipitation, followed by extraction with ether. Separation was achieved on a C18 column using ac...
journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章
doi：10.1016/s0731-7085(96)01913-9
更新日期：1997-05-01 00:00:00
abstract：:An analytical method that allows simultaneous analysis of some (semi-)volatile drugs and additives in pharmaceuticals for topical use was developed using classical static headspace as sampling technique combined with gas chromatography (HS-GC). The capillary column used, RSL-200, showed good selectivity towards all th...
journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章
doi：10.1016/j.jpba.2008.04.006
更新日期：2008-08-05 00:00:00
abstract：:Liquid chromatography-electrospray ionization tandem mass spectrometry (LC-ESIMSn) was employed to investigate the in vivo and in vitro metabolism of anisodine. Feces, urine and plasma samples were collected after ingestion of 20 mg anisodine to healthy rats. Feces and urine samples were cleaned up by liquid-liquid ex...
journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章
doi：10.1016/j.jpba.2007.01.038
更新日期：2007-07-27 00:00:00
abstract：:A micellar electrokinetic chromatography (MEKC) method for the simultaneous determination of four bioactive constituents (morroniside, loganin, paeoniflorin and paeonal) in the Chinese patent medicine Liuwei Dihuang Pills is established. A carrier composed of 0.2M boric acid, 0.02 M sodium dodecyl sulfate (SDS) and 5%...
journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章
doi：10.1016/j.jpba.2007.04.025
更新日期：2007-09-03 00:00:00
abstract：:An analytical method using electrospray ionization and high- performance liquid chromatography/tandem mass spectrometry (LC/ESI-MS/MS) was developed to quantify the vitamin B metabolites found in the folate one-carbon metabolism, using 50 μL of human plasma. Analytes in plasma were extracted using protein precipitatio...
journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章
doi：10.1016/j.jpba.2018.05.030
更新日期：2018-09-05 00:00:00
abstract：:Two UV spectrophotometric methods have been validated for the analysis of hydrolyzed tinidazole solutions. The pH of the samples must be 5.00-7.00 for both methods. The multiwavelength method may be used for samples degraded at pH 6-12 if the amount of conserved 5-nitroimidazole species is at least 93 mol.% of the ori...
journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章
doi：10.1016/s0731-7085(02)00667-2
更新日期：2003-03-10 00:00:00
abstract：:The aim of this work was to evaluate the compatibility of (+)-catechin (CA) and excipients commonly used to prepare micro and nanoemulsions using thermal analysis along with complementary assays. Lipid compounds labrasol, plurol and ethyl oleate were combined with CA according to a simplex centroid mixture design and ...
journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章
doi：10.1016/j.jpba.2017.11.069
更新日期：2018-02-05 00:00:00
abstract：:The cardiac troponin T (cTnT) is specific biomarker important for trials of acute myocardial infarctions (AMI). In this paper, a SPR sensor in real time to detect the biomarker was developed on a commercially available surface plasmon resonance AUTOLAB SPIRIT. The cTnT receptor molecule was covalently immobilized on a...
journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章
doi：10.1016/j.jpba.2006.12.013
更新日期：2007-04-11 00:00:00
abstract：:Staphylococcus aureus, methicillin-resistant Staphylococcus aureus and Klebsiella pneumoniae are the most representative bacteria causing infectious diseases. Due to the increased application of antibiotics, the bacterial resistance is growing causing severe complications. Therefore, a sensitive determination of these...
journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章
doi：10.1016/j.jpba.2016.10.025
更新日期：2017-02-05 00:00:00
abstract：:Salvianolic acid B (SAB), tanshinone IIA (TS), ginsenoside Rb₁ (Rb₁), ginsenoside Rg₁ (Rg₁) and notoginsenoside R₁ (R₁) are major active ingredients of Fufang Danshen preparation (FDP) for its protective effects on myocardial ischemia. This study investigated the pharmacokinetics of marker compounds after oral adminis...
journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章
doi：10.1016/j.jpba.2012.03.058
更新日期：2012-08-01 00:00:00
abstract：:New treatment options and improved strategies for Lysosomal Storage Disorders (LSDs) diagnosis on dried blood spot (DBS) have led to the development of several pilot newborn screening programs. Building on a previously published protocol, we devised a new 6-plex assay based on a single DBS punch incubated into a buffe...
journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章
doi：10.1016/j.jpba.2018.12.002
更新日期：2019-02-20 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：:A rapid and sensitive ultra performance liquid chromatography-tandem mass spectrometry method was developed for simultaneous determination of eight constituents, uralsaponin C, uralsaponin F, 22β-acetoxyl-glycyrrhizin, 24-hydroxy-licorice-saponin E2, licorice-saponin G2, licorice-saponin E2, glycyrrhizin, and licorice...
journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章
doi：10.1016/j.jpba.2012.11.035
更新日期：2013-03-05 00:00:00
abstract：:A reversed-phase high-performance liquid chromatography (HPLC) method with dual optical rotation/UV absorbance detection has been developed for the determination of enantiomeric purity of ephedrine hydrochloride and pseudoephedrine hydrochloride using an achiral column. The method gave a correlation coefficient of 0.9...
journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章
doi：10.1016/0731-7085(90)80050-y
更新日期：1990-01-01 00:00:00
abstract：:In this paper, the thermal stability of pure l-thyroxine (THY) and l-thyroxine sodium salt hydrate (THYSS) vs. two pharmaceutical solid formulations commercialized on both Romanian and European market (with a content of 100μg, respectively 200μg THYSS per tablet) were investigated. In order to determine whether the pr...
journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章
doi：10.1016/j.jpba.2016.03.026
更新日期：2016-06-05 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：:The development and validation of a sensitive and specific HPLC method for SDZ WAG 994 (I) in dog, monkey and rat blood is described. Sample preparation entailed double solid phase extraction (SPE) of I and the internal standard from 0.5 ml of animal blood using a phenyl and propyl sulfonic acid cation exchange column...
journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章
doi：10.1016/s0731-7085(96)01899-7
更新日期：1997-03-01 00:00:00
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：:An extracellular thermostable antibacterial peptide designated as MFAP9 was purified from marine Aspergillus fumigatus BTMF9 by ammonium sulfate precipitation followed by ion exchange chromatography on a DEAE-sepharose column. The molecular weight of MFAP9 was found to be∼3 kDa in SDS-PAGE gel corresponding a single i...
journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章
doi：10.1016/j.jpba.2020.113808
更新日期：2021-02-05 00:00:00
abstract：:The micellar electrokinetic capillary chromatography (MEKC) separation and analysis of voriconazole and UK 115794 (internal standard) were examined and an assay for determination of voriconazole in human plasma and serum was developed. The MEKC medium comprises a 2:15 (v/v) mixture of methanol and a pH 9.3 buffer comp...
journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章
doi：10.1016/j.jpba.2010.05.015
更新日期：2010-12-15 00:00:00
abstract：:A simple and rapid spectrophotometric assay is described for bronopol determination in raw material. The method is based on the measurement of absorbance (at 244 nm) of bromonitroethanol (sodium salt of aci-form), the chromophoric derivative formed from bronopol instantaneously by a retroaldol reaction in the presence...
journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章
doi：10.1016/0731-7085(96)01779-7
更新日期：1996-08-01 00:00:00
abstract：:Antioxidant therapy has been proposed to improve the oxidative stress status of diabetic patients. Natural products are a source of substances such as carotenoids, with known antioxidant properties with possible benefits on diabetes. Among them, Dunaliella salina is a microalga with high content in carotenoids that ca...
journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章
doi：10.1016/j.jpba.2008.12.041
更新日期：2009-04-05 00:00:00
abstract：:This manuscript reports the usefulness of the determination of sulphathiazole (ST) using photochemically induced fluorescence (RTPF) and RTPF coupling with first derivative (D1-RTPF), and the determination of sulphanilamide (SAN) by meaning first derivative of the emission spectrum. By irradiating 5 min, with intense ...
journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章
doi：10.1016/j.jpba.2004.12.024
更新日期：2005-06-15 00:00:00
abstract：:Botulinum type A toxin (BoNT/A) is defined by its specific endopeptidase cleavage of SNAP25 between Gln(197) and Arg(198) under reducing conditions. The neurotoxin is widely used for therapeutic or cosmetic purposes, but should not contain other toxin serotypes or unwanted protease activities. Using a neoepitope endop...
journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章
doi：10.1016/j.jpba.2010.08.013
更新日期：2011-01-05 00:00:00
abstract：:A reversed-phase ion pair liquid chromatographic method (RP-LC) for the determination of dehydroascorbic acid (DHA) and ascorbic acid (AA) and also acetaminophen, which is combined in pharmaceuticals, is proposed and validated. AA and acetaminophen were analyzed directly, while DHA was determined after pre-column deri...
journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章
doi：10.1016/j.jpba.2008.01.026
更新日期：2008-09-29 00:00:00
abstract：:Co-crystallization brings new opportunities for improving the solubility and dissolution rate of drugs with the chance of finely tuning some relevant chemical-physical properties of mixtures containing bioactive compounds. As co-crystallization process involves several molecular species, which are generally solid at r...
journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章
doi：10.1016/j.jpba.2013.01.042
更新日期：2013-05-05 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
