Article (Scientific journals)
Automatic Determination of Diltiazem and Desacetyldiltiazem in Human Plasma Using Liquid-Solid Extraction on Disposable Cartridges Coupled to Hplc--Part I: Optimization of the Hplc System and Method Validation
Hubert, Philippe; Chiap, Patrice; Crommen, Jacques
1991In Journal of Pharmaceutical and Biomedical Analysis, 9 (10-12), p. 877-882
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Abstract :
[en] A sensitive and automated method for the analysis of diltiazem and desacetyldiltiazem in plasma has been developed using liquid-solid extraction (LSE) on disposable extraction cartridges (DECs) in combination with HPLC. After isolation from plasma, the analytes are separated on a highly deactivated octyl silica column with a mobile phase of methanol-0.05 M phosphate buffer (pH 7.4) (62:38, v/v). The analytes are monitored photometrically at 238 nm. The complete preparation of the plasma sample as well as the injection of the final extract on to the analytical column are performed automatically by means of a sample processor equipped with a robotic arm to which is attached a needle dispensing the different liquids. The internal standard solution is first added to the plasma sample. The DEC is then conditioned successively with methanol and phosphate buffer (pH 7.4). A 1.0-ml volume of sample containing the internal standard solution is applied on an extraction cartridge filled with cyanopropyl silica (50 mg). After the DEC has been washed with the same buffer, the analytes are eluted with 0.16 ml of methanol. A 0.14-ml volume of buffer is then passed through the DEC and 0.25 ml of the final extract is injected onto the HPLC column. The absolute recoveries of the drugs are about 90% and the limit of detection for diltiazem is 0.8 ng ml-1. Relative standard deviations of 2.6% (within-day) and 3.7% (between-day) have been obtained for this compound at a plasma concentration of 50 ng ml-1.
Disciplines :
Pharmacy, pharmacology & toxicology
Author, co-author :
Hubert, Philippe  ;  Université de Liège - ULiège > Chimie analytique
Chiap, Patrice ;  Université de Liège - ULiège > Département de pharmacie > Analyse des médicaments
Crommen, Jacques ;  Université de Liège - ULiège > Département de pharmacie > Analyse des médicaments
Language :
English
Title :
Automatic Determination of Diltiazem and Desacetyldiltiazem in Human Plasma Using Liquid-Solid Extraction on Disposable Cartridges Coupled to Hplc--Part I: Optimization of the Hplc System and Method Validation
Publication date :
1991
Journal title :
Journal of Pharmaceutical and Biomedical Analysis
ISSN :
0731-7085
eISSN :
1873-264X
Publisher :
Elsevier, Amsterdam, Netherlands
Volume :
9
Issue :
10-12
Pages :
877-882
Peer reviewed :
Peer Reviewed verified by ORBi
Available on ORBi :
since 19 February 2009

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