Determination of enantiomers of 1-benzyl-4-[(5,6-dimethoxy-1-indanon)-2-yl]methylpiperidine hydrochloride (E2020), a centrally acting acetylcholine esterase inhibitor, in plasma by liquid chromatography with fluorometric detection

Haginaka, Jun; Seyama, Chikako

doi:10.1016/0378-4347(92)80602-m

Cited by 23 publications

(26 citation statements)

References 7 publications

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“…For the determination of donepezil in human plasma, number of methods based on high-performance liquid chromatography (HPLC) (Yasui-Furukori et al, 2002;Mihara et al, 1993;Mahasen et al, 2006;Lee et al, 1992;Matsui et al, 1999a;Haginaka and Scyama, 1992;Nakashima et al, 2006) and liquid chromatographymass spectrometry (Matsui et al, 1995(Matsui et al, , 1999b(Matsui et al, , 2006Lu Y et al, 2004;Hao et al, 2003;Apostolou et al, 2007) have been described in recent years. The majority of these methods are based on liquidliquid extraction (LLE) using isopropyl alcohol:hexane (3:97, v/v).…”

Section: Introductionmentioning

confidence: 99%

A rapid and specific approach for direct measurement of donepezil concentration in human plasma by LC‐MS/MS employing solid‐phase extraction

Shah

Kundlik

Pandya

et al. 2008

Biomedical Chromatography

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A selective, rapid and simple liquid chromatography-tandem mass spectrometry (LC-MS/MS) method is described for assay of donepezil in human plasma using escitalopram as an internal standard. Chromatographic separation was achieved on a Betabasic-C(8), 5 microm, 100 x 4.6 mm column using methanol:water:formic acid (90:9.97:0.03, v/v/v) as mobile phase. Detection of donepezil and internal standard was achieved by ESI MS/MS in positive ion mode using 380.20/91.10 and 325.13/262.00 transitions, respectively. The linearity over the concentration range of 0.15-50 ng/mL for donepezil was obtained and the lower limit of quantification was 0.15 ng/mL. For each level of quality control samples, inter-day and intra-day precisions (RSD) were < or =8.92 and 10.35% and accuracy (%RE) were < or =7.33% and 9.33%, respectively. The recovery was more than 88.50% for both donepezil and internal standard by solid-phase extraction, eliminating evaporation and reconstitution steps.

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Section: Introductionmentioning

confidence: 99%

A rapid and specific approach for direct measurement of donepezil concentration in human plasma by LC‐MS/MS employing solid‐phase extraction

Shah

Kundlik

Pandya

et al. 2008

Biomedical Chromatography

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“…8) Determination of enantiomers of Donepezil Hydrochloride in rat plasma by liquid chromatography with fluorimetric detection of I with excitation at 318 nm and emission at 390 nm was described by Haginaka and Seyama. 9) Donepezil Hydrochloride was found to be stable in acid and alkaline medium, but liable to oxidative degradation using hydrogen peroxide.…”

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confidence: 99%

Stability Indicating Methods for Determination of Donepezil Hydrochloride According to ICH Guidelines

Abbas

Fayez

Fattah

2006

CHEMICAL & PHARMACEUTICAL BULLETIN

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It is a reversibly inhibitor of acetylcholinesterase, indicated for the treatment of mild to moderate dementia of Alzheimer's type 1. The structural formula of Donepezil Hydrochloride is as follows:A few methods have been reported for the determination of I including HPLC methods in tablets 2) and human plasma.3-7) Isocratic HPLC method with fluorescence detection at 390 nm with an excitation at 325 nm for determination of donepezil in plasma and microdialysate samples was developed. 3) Analysis and enantioresolution of Donepezil was performed using capillary electrophoresis. 8) Determination of enantiomers of Donepezil Hydrochloride in rat plasma by liquid chromatography with fluorimetric detection of I with excitation at 318 nm and emission at 390 nm was described by Haginaka and Seyama. 9) Donepezil Hydrochloride was found to be stable in acid and alkaline medium, but liable to oxidative degradation using hydrogen peroxide.2) Reviewing the literature in hand, it is obvious that no spectroscopic study has been attempted to determine donepezil hydrochloride in the presence of its oxidative degradate.Upon scanning the absorption spectra of each I and II, it was observed that I has l max at 315 nm, at this wavelength II has a very little constant absorbance. Trials to use zero order absorption at 315 nm for determination of I in presence of II was successful for up to 70% of II. Zero order solve the problem of overlapping bands of I and II to certain extent but derivative spectrophotometry is a well established technique that is able to enhance the resolution of overlapping bands so to increase the selectivity of the method. D 1 and D 2 methods were constructed by measuring I at 332.1 nm and 340 nm (zero crossing of II), respectively. Different parameters affecting the D 1 and D 2 spectra were studied; namely Dl interval and smoothing factor. The best condition was by using 4 nm and 8 nm Dl interval for D 1 and D 2, respectively, without smoothing.The scientific novelty of the present work is that the methods used are simple, rapid, sensitive, and less expensive and less time consuming compared with other published LC methods. In addition, the aim of this work is to develop simple stability indicating methods for determination of I in presence of its oxidative degradate (II). ExperimentalInstrumentation A double beam UV-Visible spectrophotometer (SHI-MADZU, Japan) model UV-1601 PC with quartz cell of 1 cm path length, connected to IBM compatible computer and HP 680 inkjet printer. The bundled software was UVPC personal spectroscopy software version 3.7. The spectra bandwidth was 2 nm and wavelength-scanning speed 2800 nm/min. A spectrofluorimeter (SHIMADZU, Japan) model RF-1501 with an Epson Lx-300ϩPrinter. 1 cm quartz cell was used at low sensitivity and 2.5 nm bandwidth. TLC glass plates precoated with silica gel G F 254 (E. Merck). 25-ml Hamilton syringe. Chromatographic tank 20ϫ21ϫ9 cm (Desaga). SHI-MADZU Dual wavelength flying spot scanner, densitometer model CS9000.Materials and Reagents Donepezil Hydroc...

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“…In 1992, Haginaka and Seyama [9] reported the resolution of DPZ enantiomers in rat plasma by HPLC using a protein-based stationary phase (ovomucoid, Ultron ES-OVM) and protein precipitation for sample preparation. Matsui et al [10] developed an HPLC method for the enantioselective determination of DPZ enantiomers in dog plasma with a protein-based stationary phase (avidin, Bioptick AV-1) and direct plasma injection by column-switching procedure.…”

Section: Introductionmentioning

confidence: 99%

Chiral HPLC analysis of donepezil, 5-O-desmethyl donepezil and 6-O-desmethyl donepezil in culture medium: application to fungal biotransformation studies

et al. 2012

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An high performance liquid chromatography (HPLC) method for the enantioselective determination of donepezil (DPZ), 5-O-desmethyl donepezil (5-ODD), and 6-O-desmethyl donepezil (6-ODD) in Czapek culture medium to be applied to biotransformation studies with fungi is described for the first time. The HPLC analysis was carried out using a Chiralpak AD-H column with hexane/ethanol/methanol (75:20:5, v/v/v) plus 0.3 % triethylamine as mobile phase and UV detection at 270 nm. Sample preparation was carried out by liquid-liquid extraction using ethyl acetate as extractor solvent. The method was linear over the concentration range of 100-10,000 ng mL(-1) for each enantiomer of DPZ (r ≥ 0.9985) and of 100-5,000 ng mL(-1) for each enantiomer of 5-ODD (r ≥ 0.9977) and 6-ODD (r ≥ 0.9951). Within-day and between-day precision and accuracy evaluated by relative standard deviations and relative errors, respectively, were lower than 15 % for all analytes. The validated method was used to assess DPZ biotransformation by the fungi Beauveria bassiana American Type Culture Collection (ATCC) 7159 and Cunninghamella elegans ATCC 10028B. Using the fungus B. bassiana ATCC 7159, a predominant formation of (R)-5-ODD was observed while for the fungus C. elegans ATCC 10028B, DPZ was biotransformed to (R)-6-ODD with an enantiomeric excess of 100 %.

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Determination of enantiomers of 1-benzyl-4-[(5,6-dimethoxy-1-indanon)-2-yl]methylpiperidine hydrochloride (E2020), a centrally acting acetylcholine esterase inhibitor, in plasma by liquid chromatography with fluorometric detection

Cited by 23 publications

References 7 publications

A rapid and specific approach for direct measurement of donepezil concentration in human plasma by LC‐MS/MS employing solid‐phase extraction

A rapid and specific approach for direct measurement of donepezil concentration in human plasma by LC‐MS/MS employing solid‐phase extraction

Stability Indicating Methods for Determination of Donepezil Hydrochloride According to ICH Guidelines

Chiral HPLC analysis of donepezil, 5-O-desmethyl donepezil and 6-O-desmethyl donepezil in culture medium: application to fungal biotransformation studies

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