Development and validation of a sensitive liquid chromatography/tandem mass spectrometry method for the determination of exemestane in human plasma

Ksycińska, Hanna; Buś-Kwaśnik, Katarzyna; Szlagowska, Anna; Rudzki, Piotr J.

doi:10.1016/j.jchromb.2011.05.015

Cited by 7 publications

(4 citation statements)

References 14 publications

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“…Assays of exemestane in human plasma have been previously reported by LC-MS/MS, [5][6][7][8] however, to the best of our knowledge, totally porous reverse phase columns were typically used for separation of exemestane from endogenous interferences in human plasma. We first used a totally porous reverse phase column, BEH C18 (1.7 μm, 2.1 mm i.d.…”

Section: Discussionmentioning

confidence: 99%

“…It is thus important to develop a simple and reliable bioanalytical assay for the determination of exemestane levels in human plasma samples. Although, analytical methods for exemestane in human plasma have been reported, [5][6][7][8] most methods used complex extraction procedures such as liquid-liquid extraction or solid phase extraction. Protein precipitation is the best option in the extraction of drugs from plasma samples in terms of high-throughput and simplicity.…”

Section: Introductionmentioning

confidence: 99%

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A simple UPLC-MS/MS assay with a core-shell column for the determination of exemestane in human plasma for clinical application

Ishii¹,

Nojiri²,

Mano

2022

Eur J Mass Spectrom (Chichester)

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Exemestane is one of the aromatase inhibitors and has been used to treat breast cancer by lowering estrogen levels. Accurate quantification of exemestane is important to set an optimal dose, and thus a simple assay for exemestane is developed by ultra-performance liquid chromatography with tandem mass spectrometer. Exemestane was extracted from human plasma samples (100 μL) by simple protein precipitation with acetonitrile/methanol (1/1, v/v). Interference peaks observed close to the elution of exemestane led us to use a core shell column for higher selectivity instead of totally porous columns. The extracts were chromatographed on CORTECS UPLC C18, under a gradient elution at a flow rate of 0.25 mL/min and detected in the selected reaction monitoring. Validation parameters were assessed in accordance with the bioanalytical guidelines using quality control samples. Exemestane in human plasma was quantifiable from 0.5 to 50 ng/mL with high extraction recovery and minimal matrix effects. Hemolyzed or hyperlipemic plasma did not impact the exemestane assay. Exemestane was stable in human plasma for 392 days at −15°C or below. The developed assay was robust and successfully applied to quantifying exemestane concentrations in human plasma to support a clinical trial.

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Section: Discussionmentioning

confidence: 99%

Section: Introductionmentioning

confidence: 99%

A simple UPLC-MS/MS assay with a core-shell column for the determination of exemestane in human plasma for clinical application

Ishii¹,

Nojiri²,

Mano

2022

Eur J Mass Spectrom (Chichester)

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“…Exemestane (EXM), chemically known as 6‐methyleneandrosta‐1,4‐diene‐3,17‐dione, is an irreversible aromatase, an enzymatic transformer of androgens to estrogens, inhibitor used in a typical breast cancer treatment. It is a steroidal aromatase inhibitor usually used as oral tablets during a hormone therapy to reduce the free estrogen derivatives . Letrozole (LTZ) (4,4′‐[1 H ‐1,2,4‐triazol‐1‐yl‐methylene]bisbenzonitrile is a nonsteroidal aromatase inhibitor used during the treatment of an estrogen‐dependent breast cancer .…”

Section: Introductionmentioning

confidence: 99%

Extraction and determination of trace amounts of three anticancer pharmaceuticals in urine by three‐phase hollow fiber liquid‐phase microextraction based on two immiscible organic solvents followed by high‐performance liquid chromatography

Nazaripour

Yamini

Bagheri

2018

J of Separation Science

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An automated three-phase hollow fiber liquid-phase microextraction based on two immiscible organic solvents followed by high-performance liquid chromatography with UV-Vis detection method was applied for the extraction and determination of exemestane, letrozole, and paclitaxel in water and urine samples. n-Dodecane was selected as the supported liquid membrane and its polarity was justified by trioctylphosphine oxide. Acetonitrile was used as an organic acceptor phase with desirable immiscibility having n-dodecane. All the effective parameters of the microextraction procedure such as type of the organic acceptor phase, the supported liquid membrane composition, extraction time, pH of the donor phase, hollow fiber length, stirring rate, and ionic strength were evaluated and optimized separately by a one variable at-a-time method. Under the optimal conditions, the linear dynamic ranges were 1.8-200 (R = 0.9991), 0.9-200 (R = 0.9987) and 1.2-200 μg/L (R = 0.9983), and the limits of detection were 0.6, 0.3, and 0.4 μg/L for exemestane, letrozole, and paclitaxel, respectively. To evaluate the capability of the proposed method in the analysis of biological samples, three different urinary samples were analyzed under the optimal conditions. The relative recoveries of the three pharmaceuticals were in the range of 91-107.3% for these three analytes.

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“…Number of methods have been employed for quantification of exemestane in samples of human urine by gas chromatography/mass spectrometry [14][15] and liquid chromatography/tandem mass spectrometry [16], in human plasma by LC-MSMS [17], in various pharmaceutical dosage forms and stability testing by HPTLC, HPLC and RP-HPLC [18][19][20][21][22]. All these methods are time-consuming and involve sophisticated instrumentation.…”

Section: Introductionmentioning

confidence: 99%

Quantification of Exemestane Accumulation During Microbial Bioconversion by TLC Image Analysis

Patil

Sharma

Banerjee

et al. 2017

Int J Pharm Pharm Sci

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Objective: The present study was aimed at developing a rapid, cost effective and accurate method for quantification of exemestane using thin layer chromatography (TLC) separation followed by image analysis and to test it for monitoring the accumulation of exemestane during microbial bioconversion. Methods:After microbial bioconversion and TLC separation of products formed, exemestane was quantified using ImageQuant TL v2003 image analysis software and the results were compared with high performance liquid chromatography (HPLC) analysis. Results:The percentage error between TLC and HPLC analyses was ranged from (-) 5.18 to (+) 5.51. Bacterial strains Arthrobacter simplex IAM 1660, Nocardia sp. MTCC 1534, Pseudomonas putida MTCC 1194 and Rhodococcus rhodochorus MTCC 291 respectively yielded 79.7 (72 h), 63.9 (72 h), 69.8 (96 h) and 83.2 (96 h) mole percent bioconversion of 6-methylene androstenedione to exemestane. Conclusion:Rhodococcus rhodochorus MTCC 291 was found to be the most suitable organism for the bioconversion and may be used to develop an eco-friendly route to replace chemical synthesis that eliminates the use of toxic chemicals and side products.

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Development and validation of a sensitive liquid chromatography/tandem mass spectrometry method for the determination of exemestane in human plasma

Cited by 7 publications

References 14 publications

A simple UPLC-MS/MS assay with a core-shell column for the determination of exemestane in human plasma for clinical application

A simple UPLC-MS/MS assay with a core-shell column for the determination of exemestane in human plasma for clinical application

Extraction and determination of trace amounts of three anticancer pharmaceuticals in urine by three‐phase hollow fiber liquid‐phase microextraction based on two immiscible organic solvents followed by high‐performance liquid chromatography

Quantification of Exemestane Accumulation During Microbial Bioconversion by TLC Image Analysis

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