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

Determination of 6-amino-2,2-dimethyl-1,3-dioxepan-5-ol by postcolumn derivatization with o... 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. http://www.deepdyve.com/assets/images/DeepDyve-Logo-lg.png Chromatographia Springer Journals

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

Chromatographia , Volume 38 (7) – Apr 1, 1994

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References (22)

Publisher
Springer Journals
Copyright
Copyright © 1994 by Friedr. Vieweg & Sohn Verlagschesellschaft mbH
Subject
Chemistry; Analytical Chemistry; Organic Chemistry; Biochemistry, general; Plant Sciences; Pharmacy; Measurement Science, Instrumentation
ISSN
0009-5893
eISSN
1612-1112
DOI
10.1007/BF02269840
Publisher site
See Article on Publisher Site

Abstract

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.

Journal

ChromatographiaSpringer Journals

Published: Apr 1, 1994

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