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 of the urinary metabolites epitiostanol sulfoxide and epitiostanol was studied using liquid chromatography/mass spectrometry (LC-MS) for doping control purposes. The use of LC-MS provided advantages over gas chromatography/mass spectrometry for detecting heat labile steroids because epitiostanol and epitiostanol sulfoxide were primarily pyrolized to 5α-androst-2-en-17β-ol. The method consists of enzymatic hydrolysis using β-glucuronidase (Escherichia coli), liquid-liquid extraction, and subsequent ultra-performance liquid chromatography/electrospray-tandem mass spectrometry. Epitiostanol sulfoxide was determined at urinary concentrations of 0.5-50ng/mL, recovery was 76.2-96.9%, and assay precision was calculated as 0.9-1.7% (intra-day) and 2.0-6.6% (inter-day). Epitiostanol was determined at urinary concentrations of 0.5-50ng/mL, recovery was 26.1-35.6% and assay precision was calculated as 4.1-4.6% (intra-day) and 3.3-8.5% (inter-day). The limits of detection for epitiostanol sulfoxide and epitiostanol were 0.05ng/mL and 0.10ng/mL, respectively. Epitiostanol sulfoxide and epitiostanol, as their gluco-conjugates, were identified in human urine after oral administration of 10mg mepitiostane. Epitiostanol sulfoxide and epitiostanol could be detected up to 48h and 24h after administration, respectively. The results showed that the detection window of epitiostanol is much shorter than that of epitiostanol sulfoxide. The LC-MS detection of urinary epitiostanol sulfoxide, a specific metabolite with a sulphur atom in its molecular structure, is likely to be able to identify the abuse of mepitiostane.
journal_name
J Pharm Biomed Analjournal_title
Journal of pharmaceutical and biomedical analysisauthors
Okano M,Sato M,Kojima A,Kageyama Sdoi
10.1016/j.jpba.2015.07.016subject
Has Abstractpub_date
2015-11-10 00:00:00pages
236-44eissn
0731-7085issn
1873-264Xpii
S0731-7085(15)30070-4journal_volume
115pub_type
杂志文章abstract::A reversed-phase high-performance liquid chromatography (RP-HPLC) method with UV-detection at room temperature has been developed for the analysis of insulin and its main degradation product, A21-desamido insulin. Octadecylsilica was used as stationary phase and a mixture of water and acetonitrile containing tetramety...
journal_title:Journal of pharmaceutical and biomedical analysis
pub_type: 杂志文章
doi:10.1016/s0731-7085(03)00336-4
更新日期:2003-09-15 00:00:00
abstract::Health Canada reported recently that medical devices containing di(2-ethylhexyl) phthalate (DEHP) should not be used in the clinical treatment of infants, young boys, pregnant women, and nursing mothers. The risk assessment of DEHP released from PVC medical devices is an important issue for hospitalized patients. In t...
journal_title:Journal of pharmaceutical and biomedical analysis
pub_type: 杂志文章
doi:10.1016/s0731-7085(03)00019-0
更新日期:2003-04-10 00:00:00
abstract::A new extraction technique based on the off-line combination of pressurized-liquid with solid-phase extraction (PLE-SPE) is described. The method was used for the extraction of bioactive phenolic acids (protocatechuic, p-hydroxybenzoic, 2,3-dihydroxybenzoic, chlorogenic, vanillic, caffeic, p-coumaric, salicylic acid),...
journal_title:Journal of pharmaceutical and biomedical analysis
pub_type: 杂志文章
doi:10.1016/j.jpba.2009.03.027
更新日期:2010-01-20 00:00:00
abstract::A new stability-indicating method based on high-performance liquid chromatography coupled to ultraviolet and evaporative light scattering detection (HPLC-UV-ELSD) was developed for the quantification of daunorubicin. This is an ion-pairing, reversed-phase method. The column was a Synergi MAX-RP C12 4 μm (150 mm × 4.6 ...
journal_title:Journal of pharmaceutical and biomedical analysis
pub_type: 杂志文章
doi:10.1016/j.jpba.2013.05.007
更新日期:2013-09-01 00:00:00
abstract::A method based on capillary electrophoresis with electrochemical detection has been developed for the separation and determination of paeoniflorin, sucrose, paeonoside, glucose, and fructose in Moutan Cortex for the first time. Effects of several important factors such as the concentration of NaOH, separation voltage,...
journal_title:Journal of pharmaceutical and biomedical analysis
pub_type: 杂志文章
doi:10.1016/j.jpba.2005.11.001
更新日期:2006-04-11 00:00:00
abstract::The level of free polysaccharide is a critical quality attribute of polysaccharide-protein conjugate vaccines. The work presented describes a simple and sensitive method for the determination of low level free polysaccharides in multiple polysaccharide-protein conjugates. The method utilizes a reverse phase (RP) colum...
journal_title:Journal of pharmaceutical and biomedical analysis
pub_type: 杂志文章
doi:10.1016/j.jpba.2019.113043
更新日期:2020-02-20 00:00:00
abstract::A rapid, sensitive and selective method for the determination of carvedilol in human plasma was developed using hydrophilic interaction liquid chromatography with tandem mass spectrometry (HILIC-MS/MS). Carvedilol and cisapride (internal standard) were extracted from human plasma with methyl tert-butyl ether at basic ...
journal_title:Journal of pharmaceutical and biomedical analysis
pub_type: 杂志文章
doi:10.1016/j.jpba.2006.12.017
更新日期:2007-06-28 00:00:00
abstract::A sensitive and specific reversed-phase high-performance liquid chromatography method with ultraviolet detection has been developed and validated for the identification and quantification of SNX-2112 in rat plasma. Following sample preparation using liquid-liquid extraction, the analytes were separated by the mobile p...
journal_title:Journal of pharmaceutical and biomedical analysis
pub_type: 杂志文章
doi:10.1016/j.jpba.2010.06.031
更新日期:2010-12-01 00:00:00
abstract::The response of tumours to adriamycin, and the cardiotoxicity of the drug, may be related to its pharmacokinetics and plasma levels. Rapid and sensitive methods of adriamycin determination in plasma and urine samples are thus needed. A comparative study shows that high-performance liquid chromatography with fluorimetr...
journal_title:Journal of pharmaceutical and biomedical analysis
pub_type: 杂志文章
doi:10.1016/0731-7085(83)80042-9
更新日期:1983-01-01 00:00:00
abstract::The objective of the study was to determine the identity of a new impurity detected in HPLC chromatograms of research samples of eptifibatide manufactured by a new process and formulated into drug product. The identification of the unknown impurity was required in order to understand the mechanism of its formation. Th...
journal_title:Journal of pharmaceutical and biomedical analysis
pub_type: 杂志文章
doi:10.1016/s0731-7085(03)00409-6
更新日期:2003-12-04 00:00:00
abstract::A sensitive, selective, and specific assay was needed to study the degradation kinetics of taurolidine and its stabilization by polyvinylpyrrolidone (PVP). The purpose of the present study was to evaluate the usefulness of the chromotropic acid method and other formaldehyde or amine derivatization methods. The methods...
journal_title:Journal of pharmaceutical and biomedical analysis
pub_type: 杂志文章
doi:10.1016/s0731-7085(97)00070-8
更新日期:1997-12-01 00:00:00
abstract::A new validated method for the identification and quantification of the sibutramine was developed by HPTLC-densitometry at 225 nm and advantages and disadvantages compared with HPLC-FLD at 225 nm emission and 316 nm excitation. Both methods were applied to the analysis of three natural slimming products in the market ...
journal_title:Journal of pharmaceutical and biomedical analysis
pub_type: 杂志文章
doi:10.1016/j.jpba.2012.02.004
更新日期:2012-05-01 00:00:00
abstract::In this study, an ultra-performance liquid chromatography/photo-diode-array/quadrupole time-of-flight mass spectrometry (UPLC-PDA-QTOFMS) based chemical profiling method was established for rapid global quality evaluation of Radix Paeoniae. By virtue of the high resolution, high speed of UPLC and the accurate mass mea...
journal_title:Journal of pharmaceutical and biomedical analysis
pub_type: 杂志文章
doi:10.1016/j.jpba.2008.11.007
更新日期:2009-02-20 00:00:00
abstract::Biosensors containing cytochrome P450cam in a didodecyldimethylammonium bromide vesicular system were prepared by cross-linking onto a glassy carbon electrode (GCE) with glutaraldehyde in the presence of bovine serum albumin. Cyclic voltammetric responses of the sensor in air-free buffer solution showed that the senso...
journal_title:Journal of pharmaceutical and biomedical analysis
pub_type: 杂志文章
doi:10.1016/s0731-7085(98)00076-4
更新日期:1998-09-01 00:00:00
abstract::Stroke is the third most common cause of death in most industrialized countries. Polygonum multiflorum (He-Shou-Wu, HSW) is one of the traditional Chinese medicines with multiple pharmacological activities which is widely used in Chinese recipe. This study aims to explore the protective effect of HSW on ischemic strok...
journal_title:Journal of pharmaceutical and biomedical analysis
pub_type: 杂志文章
doi:10.1016/j.jpba.2018.03.049
更新日期:2018-06-05 00:00:00
abstract::The interactions between gemcitabine hydrochloride (GEM) and bovine serum albumin (BSA) or human serum albumin (HSA) have been studied by spectroscopic techniques. By the analysis of fluorescence spectrum and fluorescence intensity, it was observed that the GEM has a strong ability to quench the intrinsic fluorescence...
journal_title:Journal of pharmaceutical and biomedical analysis
pub_type: 杂志文章
doi:10.1016/j.jpba.2005.11.037
更新日期:2006-05-03 00:00:00
abstract::Hair analysis is a useful tool for establishing long-term drug intake. Segmental analysis, in particular, where the hair is cut into defined segments, can potentially provide a calendar of patients' drug intake as drugs are incorporated into the growing hair through the bloodstream with an average growth rate of 1 cm ...
journal_title:Journal of pharmaceutical and biomedical analysis
pub_type: 杂志文章
doi:10.1016/j.jpba.2020.113510
更新日期:2020-10-25 00:00:00
abstract::The preparation method of metal based Indian traditional drugs involves conversion of a pure metal into its oxide by repeated high temperature calcination cycles. In this work, the effect of number of calcination cycles followed in the preparation of tin oxide based Ayurvedic drug, 'vanga bhasma' was studied by a syst...
journal_title:Journal of pharmaceutical and biomedical analysis
pub_type: 杂志文章
doi:10.1016/j.jpba.2006.03.032
更新日期:2006-06-16 00:00:00
abstract::The methyl- and ethylsulphoxide diastereoisomers (V and VI) of the corticosteroid tipredane (INN, I) have been shown to undergo further stereoselective S-oxidation to yield diastereoisomeric disulphoxides (II). Interactive computer optimisation software was employed to develop semi-preparative chromatography condition...
journal_title:Journal of pharmaceutical and biomedical analysis
pub_type: 杂志文章
doi:10.1016/s0731-7085(96)01860-2
更新日期:1996-12-01 00:00:00
abstract::A simple method for the simultaneous determination of five bioactive components (rutin, puerarin, daidzein esculin and esculetin) in traditional medicinal preparations by non-aqueous capillary electrophoresis with UV detection has been developed for the first time. A running buffer composed of 15% acetonitrile, 2.5% a...
journal_title:Journal of pharmaceutical and biomedical analysis
pub_type: 杂志文章
doi:10.1016/j.jpba.2005.03.018
更新日期:2005-09-01 00:00:00
abstract::A high-performance liquid chromatographic method for the determination of the theophylline solubilizer salicylamide-O-acetic acid has been developed in the range 0.5 to 10 microg/ml for human serum and 5 to 400 microg/ml for urine. Reversed-phase ion-pair chromatography was employed with tetrabutylammonium hydrogen su...
journal_title:Journal of pharmaceutical and biomedical analysis
pub_type: 杂志文章
doi:10.1016/0731-7085(85)80062-5
更新日期:1985-01-01 00:00:00
abstract::Three impurities were detected in the LC/MS analysis of fluconazole bulk drug substance. Two of the impurities were unknowns having not been reported previously. Structural assignment of these impurities was carried out by LC/MS/MS using electrospray ionization source and an ion trap mass analyzer. Structural elucidat...
journal_title:Journal of pharmaceutical and biomedical analysis
pub_type: 杂志文章
doi:10.1016/j.jpba.2006.04.012
更新日期:2006-09-26 00:00:00
abstract::A method for the determination of cocaine (COC) and benzoylecgonine (BZE) in human urine using a column-switching liquid chromatography system is reported. A homemade precolumn (20 mm x 4.6 mm i.d.) dry-packed with Alltech ODS-C18 (35-750 microm) was employed as an extraction precolumn in order to extract and concentr...
journal_title:Journal of pharmaceutical and biomedical analysis
pub_type: 杂志文章
doi:10.1016/j.jpba.2004.09.048
更新日期:2005-02-07 00:00:00
abstract::Icariin, the major flavonoid constituent of the traditional Chinese medicine Epimedii Folium, is extensively researched owing to its comprehensive beneficial effects. This study aimed at identifying the in vivo metabolites and the metabolic profiling in rats after oral administration at a dose of icariin (100 mg/kg) w...
journal_title:Journal of pharmaceutical and biomedical analysis
pub_type: 杂志文章
doi:10.1016/j.jpba.2019.02.021
更新日期:2019-05-10 00:00:00
abstract::The chromatographic behaviour (retention, selectivity, peak shape and resolution) of seven tricyclic antidepressants (TCAs), amitryptiline, clomipramine, doxepin, imipramine, maprotiline, nortryptiline and trimipramine, was examined. Conventional unendcapped Cs and C18 columns and an endcapped XTerra MS C18 column rec...
journal_title:Journal of pharmaceutical and biomedical analysis
pub_type: 杂志文章
doi:10.1016/s0731-7085(03)00048-7
更新日期:2003-04-24 00:00:00
abstract::Extemporaneous oral preparations are routinely compounded in the pharmacy due to a lack of suitable formulations for special populations. Such small-scale pharmacy preparations also present an avenue for individualized pharmacotherapy. Orodispersible films (ODF) have increasingly been evaluated as a suitable dosage fo...
journal_title:Journal of pharmaceutical and biomedical analysis
pub_type: 杂志文章
doi:10.1016/j.jpba.2017.11.068
更新日期:2018-02-20 00:00:00
abstract::A highly sensitive and selective liquid chromatography-tandem mass spectrometry method for the determination of tetrahydrocannabinol (THC), cannabidiol, and rimonabant in rat plasma was developed. Analytes and the internal standard were extracted from plasma using a combination of protein precipitation followed by liq...
journal_title:Journal of pharmaceutical and biomedical analysis
pub_type: 杂志文章
doi:10.1016/j.jpba.2018.07.004
更新日期:2018-10-25 00:00:00
abstract::Derivatization of the free cys3,4 in human albumin, which is reported to occur under physiological conditions, has been performed in vitro by reaction of the protein with ethacrynic acid. This modification has been investigated by mass spectrometry and circular dichroism. Ethacrynic acid has been proven to bind human ...
journal_title:Journal of pharmaceutical and biomedical analysis
pub_type: 杂志文章
doi:10.1016/s0731-7085(98)00163-0
更新日期:1998-10-01 00:00:00
abstract::The current position with respect to the expression of biological potency and chemical purity of antibiotics is reviewed. In particular, attention is drawn to the policies adopted in the USA which have been a source of confusion regarding the expression of biological potency. It is suggested that the opportunity provi...
journal_title:Journal of pharmaceutical and biomedical analysis
pub_type: 杂志文章
doi:10.1016/0731-7085(87)80037-7
更新日期:1987-01-01 00:00:00
abstract::Dihydropyridine (DHP) derivatives, as calcium channel blockers with cardiovascular activity, are highly photosensitive and converted in the presence of light to compounds that are inactive. In this work, a self-modeling curve resolution method was applied to study the photodegradation kinetics of nitrendipine and felo...
journal_title:Journal of pharmaceutical and biomedical analysis
pub_type: 杂志文章
doi:10.1016/j.jpba.2007.11.020
更新日期:2008-02-13 00:00:00