Enantioselective HPLC determination and pharmacokinetic study of secnidazole enantiomers in rats

Du, Jiangbo; Zhang, Yifan; Chen, Yao; Li, Wei; Chen, Xiaoyan; Zhong, Dafang

doi:10.1016/j.jchromb.2014.06.036

Cited by 15 publications

(3 citation statements)

References 17 publications

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“…Compared to some other methods, the UPLC method has some advantages; primarily that it could remove potential interferences more efficiently than HPLC [19]. A UPLC-MS equipped with a RRHD Eclipse Plus C18 column demonstrated higher performance than HPLC and could significantly reduce the retention time [20].…”

Section: Resultsmentioning

confidence: 99%

A rapid and sensitive UPLC-MS/MS method for the determination of flibanserin in rat plasma: application to a pharmacokinetic study

You

Wang

et al. 2019

BMC Chemistry

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Background In this work, we aim to develop and validate a fast, simple, and sensitive method for the quantitative determination of flibanserin and the exploration of its pharmacokinetics. Methods Ultra-performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS) was the method of choice for this investigation and carbamazepine was selected as an internal standard (IS). The plasma samples were processed by one-step protein precipitation using acetonitrile. The highly selective chromatographic separation of flibanserin and carbamazepine (IS) was realised using an Agilent RRHD Eclipse Plus C18 (2.1 × 50 mm, 1.8 µ) column with a gradient mobile phase consisting of 0.1% formic acid in water and acetonitrile. The analytes were detected using positive-ion electrospray ionization mass spectrometry via multiple reaction monitoring (MRM). The target fragment ions were m/z 391.3 → 161.3 for flibanserin and m/z 237.1 → 194 for carbamazepine (IS). The method was validated by linear calibration plots over the range of 100–120,000 ng/mL for flibanserin (R 2 = 0.999) in rat plasma. Results The extraction recovery of flibanserin was in the range of 91.5–95.8%. The determined inter- and intra-day precision was below 12.0%, and the accuracy was from − 6.6 to 12.0%. No obvious matrix effect and astaticism was observed for flibanserin. The target analytes were long-lasting and stable in rat plasma for 12 h at room temperature, 48 h at 4 °C, 30 days at − 20 °C, as well as after three freeze–thaw cycles (from − 20 °C to room temperature). The proposed method has been fully validated and successfully applied to the pharmacokinetic study of flibanserin.

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Section: Resultsmentioning

confidence: 99%

A rapid and sensitive UPLC-MS/MS method for the determination of flibanserin in rat plasma: application to a pharmacokinetic study

You

Wang

et al. 2019

BMC Chemistry

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“…Efficient removal of proteins and other potential interference in the bio‐samples prior to LC‐MS analysis was a crucial step in the development of this method (Du et al ., , ; Ma et al ., , ). Liquid–liquid extraction by ethyl acetate, ethyl ether and chloroform was tried at first; however, their recovery (between 70.6 and 90.3%) was not very good.…”

Section: Discussionmentioning

confidence: 99%

“…Long‐term stability was assessed after storage of the standard spiked plasma samples at −20 °C for 20 days. The stability of the IS (50 ng/mL) was evaluated similarly (Du et al ., , ; Liu et al ., ).…”

Section: Methodsmentioning

confidence: 99%

Determination and validation of hupehenine in rat plasma by UPLC‐MS/MS and its application to pharmacokinetic study

Wen

Wang

Huang

et al. 2015

Biomedical Chromatography

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In this work, a sensitive and selective ultra-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) method for determination of hupehenine in rat plasma was developed and validated. After addition of imperialine as an internal standard (IS), protein precipitation by acetonitrile-methanol (9:1, v/v) was used to prepare samples. Chromatographic separation was achieved on a UPLC BEH C18 column (2.1 × 100 mm, 1.7 µm) with 0.1% formic acid and acetonitrile as the mobile phase with gradient elution. An electrospray ionization source was applied and operated in positive ion mode; multiple reaction monitoring mode was used for quantification using target fragment ions m/z 416.3 → 98.0 for hupehenine, and m/z 430.3 → 138.2 for IS. Calibration plots were linear throughout the range 2-2000 ng/mL for hupehenine in rat plasma. Mean recoveries of hupehenine in rat plasma ranged from 92.5 to 97.3%. Relative standard deviations of intra-day and inter-day precision were both <6%. The accuracy of the method was between 92.7 and 107.4%. The method was successfully applied to a pharmacokinetic study of hupehenine after either oral or intravenous administration. For the first time, the bioavailability of hupehenine was reported as 13.4%.

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Enantioselective Separation and Pharmacokinetics of a Chiral 1,4‐Dihydropyrimidine Derivative in Rats: A Combined Chromatography and Docking Approach

Sri,

Faizan,

Chandra

et al. 2024

Chirality

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Chirality in 1,4‐Dihydropyrimidines influences their pharmacological properties and synthetic strategies. Enantiomers of chiral drugs often exhibit different pharmacokinetic profiles. Therefore, separating and studying individual enantiomers is crucial to optimize drug efficacy and safety. Enantiomeric separation of ±4‐(4‐chlorophenyl)‐6‐methyl‐2‐oxo‐N‐(O‐toyl)‐1,2,3,4‐tetrahydropyrimidine‐5‐carboxamide (DP‐1), which is a 1,4‐Dihydropyrimidine derivative is achieved on CHIRALCEL® OD‐H column (particle size: 5 μm, inner diameter: 4.6 mm, length:150 mm), following by investigating the kinetic properties of (R) and (S) enantiomers. The separation was achieved with a mobile phase composed of 70% (v/v) isopropyl alcohol and 30% (v/v) n‐hexane. For the bioanalytical study, acetonitrile was used to precipitate the rat plasma samples and validated the method according to USFDA guidelines. The validated bioanalytical method was then successfully applied to determine the pharmacokinetic parameters of the drug in biological samples. Molecular modeling techniques, specifically docking simulations, were employed to predict the elution order of DP‐1 enantiomers. The docking results revealed moderate binding interactions between the enantiomers and the chiral stationary phase (CSP), which aligns with the theoretical expectation that stronger interactions lead to longer retention times on the column.

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Enantioselective HPLC determination and pharmacokinetic study of secnidazole enantiomers in rats

Cited by 15 publications

References 17 publications

A rapid and sensitive UPLC-MS/MS method for the determination of flibanserin in rat plasma: application to a pharmacokinetic study

A rapid and sensitive UPLC-MS/MS method for the determination of flibanserin in rat plasma: application to a pharmacokinetic study

Determination and validation of hupehenine in rat plasma by UPLC‐MS/MS and its application to pharmacokinetic study

Enantioselective Separation and Pharmacokinetics of a Chiral 1,4‐Dihydropyrimidine Derivative in Rats: A Combined Chromatography and Docking Approach

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