Abstract：
:The contamination of commonly used supplements by unknown steroids as well as their metabolites (parent compounds) become a challenge for the analytical laboratories. Although the determination of steroids profile is not trivial because of the complex matrix and low concentration of single compound, one of the most difficult current problem is to distinguish, during analytical procedure, endogenous androgens such as testosterone, dehydrotestosterone or dehydroepiandrosterone from their synthetic equivalents. The aim of this work was to develop and validate an analytical procedure for determination of the steroid profile in human urine by gas chromatography-combustion-isotope ratio mass spectrometry (GC/C/IRMS) toward distinguishing between endogenous and exogenous steroids. Beside the optimization of the experimental parameters for gas chromatography separation and mass spectrometry, attention was focused on urine sample preparation. Using an optimized sample preparation protocol it was possible to achieve better chromatographic resolutions and better sensitivity enabling the determination of 5 steroids, androsterone, etiocholanolone, testosterone, 5-androstandiol, 11-hydroxyandrdostane, pregnandiol, with the expanded uncertainty (k=2) below 1‰. This enable to evaluate the significant shift of the δ(13)C/(12)C [‰] values for each of examined steroids (excluding ERC). The analytical protocol described in this work was successfully used for the confirmation of positive founding urine by evaluation T/E ratio after GC/C/IRMS analysis.
journal_name
J Pharm Biomed Analjournal_title
Journal of pharmaceutical and biomedical analysisauthors
Bulska E,Gorczyca D,Zalewska I,Pokrywka A,Kwiatkowska Ddoi
10.1016/j.jpba.2014.11.017subject
Has Abstractpub_date
2015-03-15 00:00:00pages
159-66eissn
0731-7085issn
1873-264Xpii
S0731-7085(14)00544-5journal_volume
106pub_type
杂志文章abstract：:Protein modification generally occurs by addition to the amino acid side-chains of protein at the post-translational stage, for example, by enzymatic or chemical reactions after polypeptide synthesis. Recently, the recombinant hirudin analog CX-397, a potent thrombin inhibitor, was found to contain methylated Ile resi...
journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章,评审
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abstract：:Structured nanoparticles (NPs) with controlled size distribution and novel physicochemical features present fundamental advantages as drug delivery systems with respect to bulk drugs. NPs can transport and release drugs to target sites with high efficiency and limited side effects. Regulatory institutions such as the ...
journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章,评审
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doi：10.1016/s0731-7085(96)01745-1
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abstract：:The phenolic composition of herbal tea (HT) and hydromethanolic extract (HME) obtained from Grindelia robusta Nutt. was studied by HPLC-DAD-ESI/MS(n). Thirty six flavonoids and hydroxycinnamic acids were detected, from which thirty are described for the first time in this species. Quantification by HPLC-DAD showed tha...
journal_title：Journal of pharmaceutical and biomedical analysis
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doi：10.1016/j.jpba.2014.01.046
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abstract：:Flavors are commonly used in pharmaceutical oral solutions and oral suspensions to mask drug bitterness and to make the formulation more palatable. Flavor analysis during product development is typically performed by human organoleptic analysis, which is often expensive and less objective. A novel approach using a met...
journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章
doi：10.1016/s0731-7085(03)00651-4
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abstract：:Microcolumn techniques involving pre-column concentration and post-column derivatization make good use of micro-scale high-performance liquid chromatography. The efficient use of microcolumns is illustrated by some applications to the analysis of amino acids, bile acids and catecholamines. The potential of new detecto...
journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章
doi：10.1016/0731-7085(84)80073-4
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abstract：:A variety of hallucinogens of the lysergamide type has emerged on the drug market in recent years and one such uncontrolled derivative of lysergic acid diethylamide (LSD) is 1-propionyl-LSD (1P-LSD). Due to the high potency of LSD and some of its derivatives (common doses: 50-200 μg), sensitive methods are required fo...
journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章
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journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章
doi：10.1016/j.jpba.2016.12.014
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journal_title：Journal of pharmaceutical and biomedical analysis
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journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章
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journal_title：Journal of pharmaceutical and biomedical analysis
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journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章
doi：10.1016/j.jpba.2010.01.008
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journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章
doi：10.1016/j.jpba.2009.03.001
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journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章
doi：10.1016/j.jpba.2010.01.040
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journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章
doi：10.1016/0731-7085(91)80041-7
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journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章
doi：10.1016/s0731-7085(03)00108-0
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abstract：:The nonreceptor tyrosine kinase FynB is known to be required in the induction of long-term potentiation (LTP), a cellular mechanism for learning and memory. Ligands of the FynB SH2 domain as a possible FynB activator are, thus, of great interest. In this study, a solid-phase ligand binding assay was established to mee...
journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章
doi：10.1016/s0731-7085(01)00507-6
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journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章
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journal_title：Journal of pharmaceutical and biomedical analysis
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journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章
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journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章
doi：10.1016/j.jpba.2004.11.032
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abstract：:From the reaction between l-lysine and formaldehyde, Nepsilon-formyl-L-lysine was isolated by means of ion-exchange column chromatography. The identification of Nepsilon-formyl-L-lysine was carried out by ion-exchange overpressured-layer chromatography (OPLC) and 1H NMR and 13C NMR spectroscopies. The m.p. and mixed m...
journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章
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journal_title：Journal of pharmaceutical and biomedical analysis
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journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章
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更新日期：2013-05-05 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
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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
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journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章
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journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章
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更新日期：2005-09-15 00:00:00
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journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章
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abstract：:A sensitive and simple liquid chromatography-mass spectrometry (LC-MS) method has been developed and validated for the quantification of solamargine, a steroidal glycoalkaloid, in rat plasma. Vincristine was selected as the internal standard. Sample preparation involved simple liquid-liquid extraction by ethyl acetate...
journal_title：Journal of pharmaceutical and biomedical analysis
pub_type： 杂志文章
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