Chromatographia

, Volume 38, Issue 7–8, pp 479–484 | Cite as

Determination of 6-amino-2,2-dimethyl-1,3-dioxepan-5-ol by postcolumn derivatization witho-phthalaldehyde/2-mercapto-ethanol after ion-pair chromatography

  • M. Pfeffer
  • E. Walenciak-Reddel
Originals

Summary

A high-performance liquid chromatographic method is discribed for the determination of 6-amino-2,2-dimethyl-1,3-dioxepan-5-ol using Spherisorb ODS II stationary phase and mobile phase 30:70 (v/v) methanol: aqueous 1-octane sulfonic acid. Detection was fluorimetric following postcolumn derivatization with o-phthaladehyde/2-mercaptoethanol. The procedure was applied to the analysis of aqueous solutions and microcrystalline suspensions in liquid paraffin, prepared for investigation of the toxicological profile. The method was validated for selectivity, linearity of detector response, repeatability, limit of detection and quantitation. The HPLC method was selective. The instrumental limit of detection was 0.5 ng per injection (0.05 μg mL−1). The method detection limits were 0.5 μg mL−1 aqueous solution and 5 μg mL−1 liquid paraffin suspension, the quantitation limit 0.05 mg mL−1 aqueous solution and 1.0 mg mL−1 liquid paraffin. Linearity was within 0.94–47.1 μg mL−1. Intra-assay accuracy accounted for 99–100% in the range 0.05–226 mg mL−1 aqueous solution, intra-assay precision for 2% (C.V.). For microcrystalline liquid paraffin suspensions with 1 and 250 mg mL−1 99 and 109% was found for intra-assay accuracy. Intra-assay precision was 5% (C.V.). Reliable results over a wide concentration range can be obtained. The procedure is considered valid for determination of the analyte in aqueous solution or microcrystalline paraffin oil suspensions.

Key Words

Column liquid chromatography o-Phthalaldehyde Postcolumn derivatization Fluorescence detection Validation 

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Copyright information

© Friedr. Vieweg & Sohn Verlagsgesellschaft mbH 1994

Authors and Affiliations

  • M. Pfeffer
    • 1
  • E. Walenciak-Reddel
    • 1
  1. 1.Research LaboratoriesSchering AG, BerlinBerlinGermany

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