Abstract：
:Standards are required in quantitative NMR (qNMR) to obtain accurate and precise results. In this study acetanilide was established and used as a primary standard. Six other chemicals were selected as secondary standards: 3,4,5-trichloropyridine, dimethylterephthalate, maleic acid, 3-sulfolene, 1,4-bis(trimethylsilyl)benzene, and 1,3,5-trimethoxybenzene. The secondary standards were quantified using the primary standard acetanilide. A protocol for qualification and periodic checks of these secondary standards was developed, and used for evaluation of the stability of the compounds. Periodic monitoring of purity was performed for several years. The purity was higher than 99% for all secondary standards. All standards maintained the initial purity during the time period of monitoring, with very small variations in purity (0.3-0.4%). The selected secondary standards were shown to be suitable qNMR standards and that periodic requalification of the standards by qNMR ensures reliable analytical results. These standards have been used in our laboratory for compliance testing of pharmaceutical active substances and approved medicinal products as well as for analysis of suspected illegal medicines. In total more than 1000 samples have been tested using both internal and external standardization and examples are given.
journal_name
J Pharm Biomed Analjournal_title
Journal of pharmaceutical and biomedical analysisauthors
Rundlöf T,McEwen I,Johansson M,Arvidsson Tdoi
10.1016/j.jpba.2013.09.010subject
Has Abstractpub_date
2014-05-01 00:00:00pages
111-7eissn
0731-7085issn
1873-264Xpii
S0731-7085(13)00435-4journal_volume
93pub_type
杂志文章abstract：:Methods of high sensitivity, accuracy and throughput are needed for quantitation of low level residual host cell DNA in purification process intermediates and drug substances of therapeutic proteins. In this study, we designed primer/probe sets targeting repetitive Alu repeats or Alu-equivalent sequences in the human,...
journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章
doi：10.1016/j.jpba.2014.07.037
更新日期：2014-11-01 00:00:00
abstract：:Benzodiazepines (BDZ) and z-drugs belong to the most frequently prescribed medicines worldwide used for anxiety, epilepsy and sleeping disorders. Due to their pharmacology, they have a high potential for misuse. Hair analysis is being performed for the retrospective monitoring of drug exposure. However, there is a lac...
journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章
doi：10.1016/j.jpba.2020.113151
更新日期：2020-05-10 00:00:00
abstract：:Three methods are developed for the determination of two multicomponent mixtures containing guaiphenesine (GU) with salbutamol sulfate (SL), methylparaben (MP) and propylparaben (PP) [mixture 1]; and acephylline piperazine (AC) with bromhexine hydrochloride (BX), methylparaben (MP) and propylparaben (PP) [mixture 2]. ...
journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章
doi：10.1016/j.jpba.2006.09.020
更新日期：2007-02-19 00:00:00
abstract：:An automated solid-phase extraction workstation was used to develop, characterize and validate two separate HPLC methods for quantifying drugs in plasma. Method development was facilitated by workstation functions which allowed wash solvents of varying organic composition to be mixed and tested automatically. The prec...
journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章
doi：10.1016/s0731-7085(97)00278-1
更新日期：1998-08-01 00:00:00
abstract：:In addition to its antifungal activity, clotrimazole attracts interest as an anti-inflammatory drug. In order to correlate this effect with plasma concentrations in mice, a capillary electrophoretic method was developed. Sample preparation was carried out by protein precipitation using methanol. Quantification of clot...
journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章
doi：10.1016/s0731-7085(02)00531-9
更新日期：2003-01-15 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：:An ultra-sensitive liquid chromatography tandem mass spectrometry (LC-MS/MS) assay was developed and validated to facilitate the assessment of clinical pharmacokinetics of nucleotide analogs from lysed intracellular matrix. The method utilized a strong anion exchange isolation of mono-(MP), di-(DP), and tri-phosphates...
journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章
doi：10.1016/j.jpba.2011.05.039
更新日期：2011-09-10 00:00:00
abstract：:A validated, highly sensitive and selective high-pressure liquid chromatography-tandem mass spectrometry (LC-MS/MS) method was developed for the quantitative determination of quetiapine (QUE) in human Na2EDTA plasma with mass spectrometry (MS) detection. Clozapine (CLO) was employed as an internal standard. Samples we...
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.2007.03.034
更新日期：2007-06-28 00:00:00
abstract：:There must be a large market for active pharmaceutical ingredients of illegal source to support the huge and lucrative business of trade in illegal medicines. The active substances found in illegal pharmaceuticals may differ from their legal counterparts concerning purity and associated risks for the health of the use...
journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章
doi：10.1016/j.jpba.2016.08.027
更新日期：2016-11-30 00:00:00
abstract：:An accurate and specific gas chromatography-mass spectrometry (GC-MS) method was optimized to quantify specific polyunsaturated fatty acids (PUFAs) in plasma and in erythrocyte membranes for clinical purposes. The developed and fully-validated method showed optimal linearity in addition to adequate results in terms of...
journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章
doi：10.1016/j.jpba.2019.07.012
更新日期：2019-11-30 00:00:00
abstract：:This paper describes a new liquid chromatography-tandem mass spectrometric (LC-MS/MS) method for the analysis of three stanozolol metabolites (16β-hydroxystanozolol, 3'-hydroxystanozolol, and 4β-hydroxystanozolol) in urines of animal origins. The solid-phase extraction (SPE) clean-up procedure was optimized to reduce ...
journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章
doi：10.1016/j.jpba.2013.08.019
更新日期：2014-01-01 00:00:00
abstract：:A porous zwitterionic monolithic column was prepared to rapidly and efficiently separate lysozyme from egg white. The monolith was synthesized in a stainless steel HPLC column (5 cm × 4.6 mm i.d.) by in-situ thermal initiated co-polymerization of N,N-dimethyl-N-methacryloxyethyl-N-(3-sulfopropyl) ammonium betaine (MSA...
journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章
doi：10.1016/j.jpba.2019.07.009
更新日期：2019-10-25 00:00:00
abstract：:A quick and sensitive method has been developed and validated for the determination of tungsten in bulk drug substance and intermediates using either Inductively Coupled Plasma Atomic Emission Spectrometry (ICP-AES) or Inductively Coupled Plasma Mass Spectrometry (ICP-MS). Sample preparation is by direct dissolution w...
journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章
doi：10.1016/s0731-7085(98)00259-3
更新日期：1999-05-01 00:00:00
abstract：:SU101 or leflunomide, has been studied extensively because of its anti-cancer and immunomodulating properties. The parent isoxazole compound is converted in vitro and metabolized in vivo to an open ring isomeric form, SU0020. Several pharmacological activities have been reported for the parent and metabolite compounds...
journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章
doi：10.1016/s0731-7085(01)00654-9
更新日期：2002-05-15 00:00:00
abstract：:The subject of the analysis of various elements, including metals and metalloids, in the pharmaceutical industry has seen increasing importance in the last 10-15 years, as modern analytical instrumentation has afforded analysts with the opportunity to provide element-specific, accurate and meaningful information relat...
journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章,评审
doi：10.1016/j.jpba.2010.11.030
更新日期：2011-06-25 00:00:00
abstract：:Quantitative analysis of metabolic mixtures by (1)H 1D NMR offers a limited potential for precise quantification of biomarkers, due to strong overlap between the peaks. Two-dimensional spectroscopy is a powerful tool to unambiguously and simultaneously measure a larger number of metabolite contributions. However, it i...
journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章
doi：10.1016/j.jpba.2010.07.046
更新日期：2011-01-05 00:00:00
abstract：:The objective of the work was to assess the possible interactions between the model drug diclofenac sodium (DS) and the water-insoluble ammonio methacrylate copolymer (AMC). Films with different drug/polymer ratios were therefore prepared by the solvent casting method and investigated as a preformulation study towards...
journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章
doi：10.1016/j.jpba.2007.10.008
更新日期：2008-01-22 00:00:00
abstract：:A sensitive and specific LC-MS assay for DT-13 in rat plasma was developed. DT-13 is an active steroidal saponin present in Liriopes Radix and is developed as an anti-tumor drug candidate. The samples were extracted by acetonitrile-mediated plasma protein precipitation. The chromatographic separation was carried out u...
journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章
doi：10.1016/j.jpba.2011.07.003
更新日期：2011-11-01 00:00:00
abstract：:A simple, rapid and sensitive isocratic reversed phase HPLC method with UV detection using a monolithic column has been developed and validated for the determination of gliclazide in human plasma. The assay enables the measurement of gliclazide for therapeutic drug monitoring with a minimum quantification limit of 10n...
journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 临床试验,杂志文章
doi：10.1016/j.jpba.2006.05.003
更新日期：2006-10-11 00:00:00
abstract：:In this paper, binding interaction of 5-(ethoxycarbonyl)-6-methyl-4-(4-methoxyphenyl)-3,4-dihydropyrimidin-2(1H)-one (EMMD) with human serum albumin (HSA) under physiological conditions was investigated by using spectroscopy, isothermal titration calorimetry (ITC) and molecular modeling techniques. The results of spec...
journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章
doi：10.1016/j.jpba.2011.03.006
更新日期：2011-07-15 00:00:00
abstract：:A method is described for the GC-NPD determination of urinary codeine and morphine after derivatization with trifluoroacetic anhydride. The lower limit for accurate quantitative determination was 0.05 microgram ml-1. After the oral administration of Bisolvon Griblettes corresponding to 30 mg codeine phosphate to seven...
journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章
doi：10.1016/0731-7085(93)80026-w
更新日期：1993-04-01 00:00:00
abstract：:In LC method development, the choice of suitable experimental conditions is often challenging for the analyst because of the huge diversity of stationary phases, mobile phase pH and organic modifiers, that could significantly alter the selectivity. The influence of these parameters on selectivity was experimentally te...
journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章
doi：10.1016/j.jpba.2012.01.019
更新日期：2012-04-07 00:00:00
abstract：:A method for the separation of polymerized impurities in meropenem has been developed by gel filtration chromatography (GFC). The chromatographic conditions included a Superdex peptide HR 10/30 column and the mobile phase consisting of 0.01 mol L(-1) sodium phosphate buffer (pH 7.0), at a flow rate of 0.8 mL min(-1). ...
journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章
doi：10.1016/j.jpba.2004.11.023
更新日期：2005-03-09 00:00:00
abstract：:Near-infrared (NIR) spectroscopy is one of the most successful pharmaceutical process analytical tools. For botanical drug products (BDPs), many studies have applied NIR spectroscopy for rapid analysis of botanical raw materials, extracts and formulations. However, the real-time process analysis reported for BDPs was ...
journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章
doi：10.1016/j.jpba.2019.06.046
更新日期：2019-09-10 00:00:00
abstract：:The current study assesses the effect of extending column length during gradient packed column sub/supercritical fluid chromatography (PCSFC) experiments on the detection of known and unknown impurities in a drug substance sample. Quantitative drug substance impurity profiles were generated and compared using multiple...
journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章
doi：10.1016/s0731-7085(01)00405-8
更新日期：2001-10-01 00:00:00
abstract：:Although chemotherapy is widely used to treat human cancers, most chemotherapeutic agents only benefit a small fraction of patients because of the heterogeneity of cancers. Therefore, identifying of the sensitivity of cancers toward various chemotherapies would be important for choosing of chemotherapeutic regime. In ...
journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章
doi：10.1016/j.jpba.2014.10.018
更新日期：2015-01-01 00:00:00
abstract：:Originally cultivated in the Peruvian Andes, Maca (Lepidium meyenii) is now widely consumed as functional food which is known for its functional characteristic like relieving fatigue and enhancing stamina. Macamides are the unique fatty acids with long-chain and N-benzylamides among the various constituents extracted ...
journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章
doi：10.1016/j.jpba.2018.11.041
更新日期：2019-02-05 00:00:00
abstract：:In order to facilitate correlation calculation and matrix-based resolution in comprehensive two-dimensional gas chromatography - mass spectrometry (GC × GC-MS) data-set, an intelligent clustering of modulation peaks (ICMP) algorithm was developed in this paper. ICMP is start with the second -dimension (2D) peak restri...
journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章
doi：10.1016/j.jpba.2020.113800
更新日期：2021-02-05 00:00:00
abstract：:The development and validation of an HPLC method for the quantification of eight peptide antigens from the therapeutic cancer vaccine DPX-0907 is described. The antigens were formulated in DepoVax™, a patented liposomal vaccine delivery platform used in a phase 1 study for breast, ovarian, and prostate cancers. A grad...
journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章
doi：10.1016/j.jpba.2012.03.046
更新日期：2012-07-01 00:00:00
abstract：:During routine screenings of two "libido enhancer" dietary supplements using LC-MS(n), two compounds were detected that displayed structural similarities to tadalafil. These compounds were isolated from the supplements using high-performance liquid chromatography with fraction collection, and were characterized furthe...
journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章
doi：10.1016/j.jpba.2011.09.038
更新日期：2012-02-05 00:00:00
