A validated HPLC method for the determination of donepezil in human plasma after derivatization with 9-fluorenylmethyl chloroformate

doi:10.5246/jcps.2014.02.015

中国药学(英文版)

A validated HPLC method for the determination of donepezil in human plasma after derivatization with 9-fluorenylmethyl chloroformate

Reza Ahmadkhaniha, Abdolrahman Nazari, Mohsen Amini, Effat Souri^*

1. Department of Human Ecology, School of Public Health, Tehran University of Medical Sciences, Tehran 14176-14411, Iran
2. Department of Medicinal Chemistry, Faculty of Pharmacy and Drug Design and Development Research Center, Tehran University of Medical Sciences, Tehran 14155-6451, Iran

收稿日期:2013-08-20 修回日期:2013-10-07 出版日期:2014-02-15 发布日期:2014-01-25
通讯作者: Effat Souri*
作者简介:*Corresponding author. Tel.: 98-21-66959065; Fax: 98-21-66461178; E-mail: souri@sina.tums.ac.ir

A validated HPLC method for the determination of donepezil in human plasma after derivatization with 9-fluorenylmethyl chloroformate

Reza Ahmadkhaniha, Abdolrahman Nazari, Mohsen Amini, Effat Souri^*

1. Department of Human Ecology, School of Public Health, Tehran University of Medical Sciences, Tehran 14176-14411, Iran
2. Department of Medicinal Chemistry, Faculty of Pharmacy and Drug Design and Development Research Center, Tehran University of Medical Sciences, Tehran 14155-6451, Iran

Received:2013-08-20 Revised:2013-10-07 Online:2014-02-15 Published:2014-01-25
Contact: Effat Souri*
About author:*Corresponding author. Tel.: 98-21-66959065; Fax: 98-21-66461178; E-mail: souri@sina.tums.ac.ir

摘要/Abstract

摘要：

A new HPLC method has been developed for determining donepezil in human plasma. To find the optimum conditions, a derivatization reaction was performed in different media, and the reaction product was identified by NMR and GC-MS after a semi-preparative HPLC separation. Under optimized conditions, donepezil was derivatized by 9-fluorenylmethyl chloroformate in chloroform and carbonate buffer at pH 9.5 in the presence of NaI after solid-phase extraction from a plasma sample. The reaction product was quantified on a reversed-phase TRACER EXCEL ODS-A, 5 µm column using a mixture of acetonitrile–10 mM acetate buffer (pH 6.0)–THF (60:35:5, v/v/v) as the mobile phase with fluorescence detection at 264 nm (ex) and 313 nm (em). Fluoxetine was used as the internal standard. The total run-time of the analysis was about 10 min, and a clean chromatogram was obtained. The developed method was linear over the range of 1–100 ng/mL in 500 µL of plasma samples (r²>0.998). The intra-day and inter-day precision values were in the range of 2.6%–11.6%. The limit of quantification was 1 ng/mL.

关键词: 9-Fluorenylmethyl chloroformate, Derivatization, HPLC

Abstract:

Key words: 9-Fluorenylmethyl chloroformate, Derivatization, HPLC

中图分类号:

R917

Supporting:

Reza Ahmadkhaniha, Abdolrahman Nazari, Mohsen Amini, Effat Souri. A validated HPLC method for the determination of donepezil in human plasma after derivatization with 9-fluorenylmethyl chloroformate[J]. 中国药学(英文版), DOI: 10.5246/jcps.2014.02.015.

Reza Ahmadkhaniha, Abdolrahman Nazari, Mohsen Amini, Effat Souri. A validated HPLC method for the determination of donepezil in human plasma after derivatization with 9-fluorenylmethyl chloroformate[J]. Journal of Chinese Pharmaceutical Sciences, DOI: 10.5246/jcps.2014.02.015.

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A validated HPLC method for the determination of donepezil in human plasma after derivatization with 9-fluorenylmethyl chloroformate

A validated HPLC method for the determination of donepezil in human plasma after derivatization with 9-fluorenylmethyl chloroformate

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