Article (Scientific journals)
Determination of verapamil and norverapamil in human plasma by liquid chromatography: comparison between a liquid-liquid extraction procedure and an automated liquid-solid extraction method for sample preparation.
Hubert, Philippe; Chiap, Patrice; Ceccato, Attilio et al.
1992In Journal of Pharmaceutical and Biomedical Analysis, 10 (10-12), p. 937-42
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Keywords :
Buffers; Chromatography, High Pressure Liquid; Humans; Reference Standards; Sulfuric Acids; Verapamil/analogs & derivatives/blood
Abstract :
[en] A conventional liquid-liquid extraction (LLE) procedure with high-performance liquid chromatography (HPLC) has been developed for the determination of verapamil and its main metabolite, norverapamil, in plasma. After addition of the internal standard, plasma samples were basified with phosphate buffer (pH 9.0) and extracted with a mixture of cyclohexane-dichloromethane. After centrifugation, the organic layer was separated and the analytes were extracted back into a 0.1 N sulphuric acid solution containing 2-aminoheptane. An aliquot of this aqueous phase was then injected directly onto the HPLC column. This LLE procedure has been compared with an automated liquid-solid extraction (LSE) method that has been developed in parallel. Good linearity was obtained using both extraction methods. The absolute recoveries for the two analytes were ca 95% with the automated LSE procedure and slightly lower (ca 84%) for the LLE method. The automated method gives better results with respect to detectability and precision, but the LLE procedure is simpler to develop, requires much less expensive equipment, and remains a useful alternative when the number of samples to be analysed is limited.
Disciplines :
Pharmacy, pharmacology & toxicology
Author, co-author :
Hubert, Philippe  ;  Université de Liège - ULiège > Département de pharmacie > Chimie analytique
Chiap, Patrice ;  Centre Hospitalier Universitaire de Liège - CHU > Pharmacologie clinique
Ceccato, Attilio ;  Université de Liège - ULiège > Département de pharmacie > Analyse des médicaments
Bechet, I.
Sibenaler-Dechamps, R.
Maes, P.
Crommen, Jacques ;  Université de Liège - ULiège > Département de pharmacie > Analyse des médicaments
Language :
English
Title :
Determination of verapamil and norverapamil in human plasma by liquid chromatography: comparison between a liquid-liquid extraction procedure and an automated liquid-solid extraction method for sample preparation.
Publication date :
1992
Journal title :
Journal of Pharmaceutical and Biomedical Analysis
ISSN :
0731-7085
eISSN :
1873-264X
Publisher :
Elsevier Science, Oxford, United Kingdom
Volume :
10
Issue :
10-12
Pages :
937-42
Peer reviewed :
Peer Reviewed verified by ORBi
Available on ORBi :
since 31 March 2009

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