Reference : Automatic Determination of Diltiazem and Desacetyldiltiazem in Human Plasma Using Liquid...
Scientific journals : Article
Human health sciences : Pharmacy, pharmacology & toxicology
http://hdl.handle.net/2268/7421
Automatic Determination of Diltiazem and Desacetyldiltiazem in Human Plasma Using Liquid-Solid Extraction on Disposable Cartridges Coupled to Hplc--Part II: Optimization of Liquid-Solid Extraction
English
Hubert, Philippe mailto [Université de Liège - ULg > > Chimie analytique >]
Chiap, Patrice mailto [Université de Liège - ULg > Département de pharmacie > Analyse des médicaments >]
Crommen, Jacques mailto [Université de Liège - ULg > Département de pharmacie > Analyse des médicaments >]
1991
Journal of Pharmaceutical & Biomedical Analysis
9
10-12
883-887
Yes (verified by ORBi)
0731-7085
[en] An automatic liquid-solid extraction (LSE) procedure to be coupled to HPLC for the determination of diltiazem and desacetyldiltiazem in plasma has been developed. The LSE operations are performed on disposable extraction cartridges (DECs) by means of a sample processor equipped with a robotic arm holding a needle through which the different liquids are dispensed. The operating parameters of LSE have been optimized with respect to recovery, detectability and reproducibility by using, whenever possible, aqueous solutions of the analytes. Different kinds of DECs have been tested. For the compounds studied, DECs filled with 50 mg of cyanopropyl silica have been selected. The influence of the pH of the buffer used in the washing step has been studied, leading finally to the selection of the same phosphate buffer (pH 7.4) as in the HPLC mobile phase. The minimum volume of methanol which still gives a nearly complete elution of the analytes from the extraction cartridges has been determined. Under these conditions, a high sensitivity can be obtained without an evaporation step. Moreover, the volume of buffer to be added to the methanolic eluate before injection into the HPLC system has been optimized in such a way that a focusing effect is obtained at the top of the analytical column while the dilution of the extract is minimized.
http://hdl.handle.net/2268/7421

File(s) associated to this reference

Fulltext file(s):

FileCommentaryVersionSizeAccess
Restricted access
Hubert_1991_J-Pharm-Biomed-Anal_883.pdfNo commentaryPublisher postprint324.89 kBRequest copy

Bookmark and Share SFX Query

All documents in ORBi are protected by a user license.