Development and validation of an automated solid phase extraction and liquid chromatographic method for determination of piperaquine in urine

Document identifier: oai:dalea.du.se:1623
Access full text here:10.1016/j.jpba.2005.10.027
Keyword: Natural Sciences, Chemical Sciences, Naturvetenskap, Kemi, Piperaquine; liquid chromatography; solid-phase extraction; validation; method development; Urine
Publication year: 2006
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Abstract:

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.

Authors

J. Tärning

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T. Singtoroj

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A. Annerberg

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M. Ashton

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Yngve Bergqvist

Högskolan Dalarna; Kemiteknik
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N. White

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N. Day

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N. Lindegårdh

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