Detection of new exemestane metabolites by liquid chromatography interfaced to electrospray-tandem mass spectrometry

Cavalcanti, Gustavo de Albuquerque; Garrido, Bruno Carius; Leal, Felipe Dias; Padilha, Marina; Mazzarino, Monica; Torre, Xavier de la; Botrè, Francesco; Neto, Francisco Radler de Aquino

doi:10.1016/j.jsbmb.2011.08.014

Cited by 16 publications

(10 citation statements)

References 16 publications

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“…The renamed category S4 (Hormone and metabolic modulators) includes five sub‐groups, of which the class of aromatase inhibitors (4.1) lists exemestane that was subjected to human in vivo metabolism studies . Four metabolites formerly not reported were discussed and structures were assigned and proposed based on LC‐MS and LC‐MS/MS (with accurate mass) data.…”

Section: Hormone and Metabolic Modulatorsmentioning

confidence: 99%

Annual banned‐substance review: analytical approaches in human sports drug testing

Thevis¹,

Kuuranne

Geyer

et al. 2012

Drug Testing and Analysis

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Frequently updated anti-doping regulations and detection strategies for banned substances and methods of doping are vital for efficient and scientifically substantiated abatement of drug abuse, manipulation, and illicit performance enhancement in sport. In 2012, the ninth version of the Prohibited List as annually issued by the World Anti-Doping Agency (WADA) reports on modest but relevant modifications from its 2011 predecessor. Awareness of old and new analytical challenges in sports drug testing, together with issues resulting from altered rules and regulations, have given rise to numerous research projects aiming at improved detection strategies to strengthen international anti-doping efforts. In this annual banned substance review, emerging and advancing methods in the detection of known and recently outlawed substances are reported. New and/or enhanced procedures and techniques of doping analysis are reviewed together with information relevant to doping controls. The review surveys and critiques literature published between October 2011 and September 2012.

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Section: Hormone and Metabolic Modulatorsmentioning

confidence: 99%

Annual banned‐substance review: analytical approaches in human sports drug testing

Thevis¹,

Kuuranne

Geyer

et al. 2012

Drug Testing and Analysis

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“…For GC-HRMS methods, the analytes can be isolated by procedures also used for LC but they may need proper derivatization such as trimethylsilylation for steroids depending on the analytes' structure [30]. As recently reviewed by Soederholm et al [47], microwave-assisted derivatization shortens the incubation time for derivatization before GC-MS analysis.…”

Section: Sample Preparationmentioning

confidence: 99%

“…Despite the fact that most of the modern HR mass spectrometers used for the metabolism studies were coupled to LC, GC coupled to HR mass spectrometers is still in use for investigating the metabolism of drugs, e.g., exemestane [30]. Even an OT analyzer was recently successfully coupled to a GC system [52].…”

Section: Ionization and Fragmentation Techniquesmentioning

confidence: 99%

“…Even an OT analyzer was recently successfully coupled to a GC system [52]. Using GC-MS, there is no doubt that electron impact (EI) is the most promising ionization technique for structure elucidation, whereas positive ion chemical ionization is mainly used for confirmation of molecular masses as previously shown [15,30]. Concerning LC-MS, there is still a debate whether to use ESI or atmospheric pressure chemical ionization (APCI).…”

Section: Ionization and Fragmentation Techniquesmentioning

confidence: 99%

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Current applications of high-resolution mass spectrometry in drug metabolism studies

Meyer

Maurer

2012

Anal Bioanal Chem

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This paper reviews high-resolution mass spectrometry (HRMS) approaches published in 2007-2011 for the elucidation of drug metabolism with a focus on new therapeutics, new drugs of abuse, and doping agents using time-of-flight, single-stage Orbitrap, ion trap Orbitrap, and other Fourier transform MS-based techniques. The present review provides an overview of metabolite-generating systems and assays used, sample preparation techniques, ionization and fragmentation techniques, as well as data mining strategies and software tools which were used in the reviewed papers. Furthermore, HRMS-specific topics such as demand for a certain resolution or a specific mass accuracy are discussed in detail and corresponding recommendations are given. Finally, the advantages and limitations of these methods are discussed.

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“…Literature survey reports that Exemestane can be determined by different analytical techniques such as HPTLC 5 , UV-spectrophotometry 6 , GC-MS 7 , LC-MS [8][9][10][11][12] , LC-radio immuno assay 13 , HPLC [14][15][16][17] and UPLC 18 in pharmaceutical dosage forms and in biological fluids. So far only two stability indicating HPLC [19][20] methods were reported for the determination of Exemestane and at present the authors have proposed a robust, precise and accurate stability indicating liquid chromatographic method for the determination of Exemestane in pharmaceutical dosage forms.…”

Section: Introductionmentioning

confidence: 99%

A Validated Stability-Indicating Liquid Chromatographic Method for the Determination of Exemestane

2014

Chem Sci Trans

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A stability indicating liquid chromatographic method was developed for the determination of Exemestane in presence of degradation products using Zorbax SB C18 (150 mm × 4.6 mm i. d., 3.5 µm particle size) column with a flow rate 1.2 mL/min (UV detection 247 nm). Linearity was observed over a concentration range 0.1-200 μg/mL with regression equation y = 56288 x -3004 (R 2 = 0.999). Forced degradation studies were performed and Exemestane is reported to be highly sensitive towards oxidation. The method was validated as per ICH guidelines.

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Detection of new exemestane metabolites by liquid chromatography interfaced to electrospray-tandem mass spectrometry

Cited by 16 publications

References 16 publications

Annual banned‐substance review: analytical approaches in human sports drug testing

Annual banned‐substance review: analytical approaches in human sports drug testing

Current applications of high-resolution mass spectrometry in drug metabolism studies

A Validated Stability-Indicating Liquid Chromatographic Method for the Determination of Exemestane

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