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Development and validation of an automated solid phase extraction and liquid chromatographic method for determination of piperaquine in urine
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2006 (English)In: Journal of Pharmaceutical and Biomedical Analysis, ISSN 0731-7085, E-ISSN 1873-264X, Vol. 41, no 1, p. 213-218Article in journal (Refereed) Published
Abstract [en]

A sensitive and specific bioanalytical method for determination of piperaquine in urine by automated solid-phase extraction (SPE) and liquid chromatography (LC) has been developed and validated. Buffered urine samples (containing internal standard) were loaded onto mixed phase (cation-exchange and octylsilica) SPE columns using an ASPEC XL SPE robot. Chromatographic separation was achieved on a Chromolith Performance RP-18e (100 mm × 4.6 mm I.D.) LC column with phosphate buffer (pH 2.5; 0.1 mol/L)–acetonitrile (92:8, v/v). Piperaquine was analysed at a flow rate of 3 mL/min with UV detection at 347 nm. A linear regression model on log–log transformed data was used for quantification. Within-day precision for piperaquine was 1.3% at 5000 ng/mL and 6.6% at 50 ng/mL. Between-day precision for piperaquine was 3.7% at 5000 ng/mL and 7.2% at 50 ng/mL. Total-assay precision for piperaquine over 4 days using five replicates each day (n = 20) was 4.0%, 5.2% and 9.8% at 5000, 500 and 50 ng/mL, respectively. The lower limit of quantification (LLOQ) was set to 3 ng/mL using 1 mL of urine, which could be lowered to 0.33 ng/mL when using 9 mL of urine and an increased injection volume.

Place, publisher, year, edition, pages
2006. Vol. 41, no 1, p. 213-218
Keywords [en]
piperaquine; liquid chromatography; solid-phase extraction; validation; method development; Urine
National Category
Chemical Sciences
Identifiers
URN: urn:nbn:se:du-1623DOI: 10.1016/j.jpba.2005.10.027ISI: 000236655100029PubMedID: 16311004OAI: oai:dalea.du.se:1623DiVA, id: diva2:519578
Available from: 2005-12-21 Created: 2005-12-21 Last updated: 2017-12-07Bibliographically approved

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CiteExportLink to record
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Citation style
  • apa
  • ieee
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  • nn-NB
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