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Automated solid-phase extraction method for the determination of piperaquine in whole blood by rapid liquid chromatography
Uppsala University, Disciplinary Domain of Science and Technology, Chemistry, Department of Chemistry, Analytical Chemistry.
Uppsala University, Disciplinary Domain of Science and Technology, Chemistry, Department of Chemistry, Analytical Chemistry.
2003 (English)In: Therapeutic Drug Monitoring, ISSN 0163-4356, E-ISSN 1536-3694, Vol. 25, no 5, 544-551 p.Article in journal (Refereed) Published
Abstract [en]

A bioanalytic method for the determination of piperaquine in whole blood by solid-phase extraction and rapid liquid chromatography has been developed and validated. Whole blood was hemolyzed with deionized water, and an internal standard was added to the samples before they were loaded onto a PRS cation-exchange solid-phase extraction column. Piperaquine and internal standard were analyzed by liquid chromatography on a Chromolith Performance (100 x 4.6 mm) column with mobile phase acetonitrile:phosphate buffer, I = 0.1, pH 2.5 (8:92, vol/vol), flow rate 4 mL x min-1, and UV detection at 345 nm. The intraassay precision for whole blood was 3.2% at 3.00 microM and 12.3% at 0.100 microM. The interassay precision for whole blood was 1.8% at 3.00 microM and 5.2% at 0.100 microM. The lower limit of quantification and the limit of detection were 0.050 microM and 0.010 microM, respectively.

Place, publisher, year, edition, pages
2003. Vol. 25, no 5, 544-551 p.
National Category
Natural Sciences
Identifiers
URN: urn:nbn:se:uu:diva-90192PubMedID: 14508376OAI: oai:DiVA.org:uu-90192DiVA: diva2:162458
Available from: 2003-04-24 Created: 2003-04-24 Last updated: 2013-06-19Bibliographically approved
In thesis
1. Development of Field-adapted Analytical Methods for the Determination of New Antimalarial Drugs in Biological Fluids
Open this publication in new window or tab >>Development of Field-adapted Analytical Methods for the Determination of New Antimalarial Drugs in Biological Fluids
2003 (English)Doctoral thesis, comprehensive summary (Other academic)
Abstract [en]

This thesis deals with the development of analytical methods for the determination of new antimalarial drugs in biological fluids. The goal was to develop methods that facilitate clinical studies performed in the field, such as capillary blood sampling onto sampling paper.

Methods for the determination of atovaquone (ATQ) in plasma, whole blood and capillary blood applied onto sampling paper were developed and validated.

Automated solid-phase extraction (SPE) and liquid chromatography (LC) with UV absorbance detection was used to quantify ATQ. Venous blood contained higher levels of ATQ than capillary blood after a single dose of Malarone (ATQ + proguanil).

Ion-pairing LC was used to separate amodiaquine (AQ), chloroquine (CQ) and their metabolites on a CN-column. A method for quantification of AQ, CQ and their metabolites in capillary blood applied onto sampling paper was developed and validated. Perchloric acid and acetonitrile were used to facilitate the extraction of the analytes from the sampling paper. The liquid extract was further cleaned by SPE.

Methods for the determination of piperaquine (PQ) in plasma and whole blood using SPE and LC were developed and validated. Addition of trichloroacetic acid (TCA) to the samples prior to injection into the LC-system significantly enhanced the efficiency for the PQ peak. Serum and whole blood contained higher levels (about 300 nM) of PQ than plasma (about 200 nM) after a single oral dose of 340 mg PQ. This indicates that PQ may be taken up in the leucocytes and thrombocytes.

Place, publisher, year, edition, pages
Uppsala: Acta Universitatis Upsaliensis, 2003. 64 p.
Series
Comprehensive Summaries of Uppsala Dissertations from the Faculty of Science and Technology, ISSN 1104-232X ; 823
Keyword
Analytical chemistry, LC, liquid chromatography, biological samples, SPE, solid phase extraction, validation, antimalarial drugs, amodiaquine, piperaquine, atovaquone, dried blood spots, Analytisk kemi
National Category
Analytical Chemistry
Research subject
Analytical Chemistry
Identifiers
urn:nbn:se:uu:diva-3346 (URN)91-554-5573-5 (ISBN)
Public defence
2003-05-16, Teknikdalens Aula, Teknikdalen, Borlänge, Borlänge, 13:15
Opponent
Supervisors
Available from: 2003-04-24 Created: 2003-04-24Bibliographically approved

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