Qualitative Thin-Layer and High-Performance Liquid Chromatographic Analysis of 1-Substituted Diazen- 1-ium-1,2-diolates on Aminopropyl-Bonded Silica Gel
✍ Scribed by Anthony L. Fitzhugh; Nwanne O. Anadu; David J. Waterhouse; Joseph A. Hrabie; Joseph E. Saavedra; Larry K. Keefer
- Publisher
- Elsevier Science
- Year
- 2002
- Tongue
- English
- Weight
- 112 KB
- Volume
- 301
- Category
- Article
- ISSN
- 0003-2697
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✦ Synopsis
High-performance liquid (HPLC) and thin-layer (TLC) chromatographic methods for the detection and quantification of diazeniumdiolates are described. The HPLC determinations were made using a Rocket Platinum NH 2 column (7 ؋ 53 mm, 100-Å pore size, 3-m particle size), under isocratic conditions with mixtures of acetonitrile, methanol, and water containing 0.1% diethylamine (v/v), at a flow rate of 2.5 ml/min, a column temperature of 22°C, and UV detection at 250 nm. The TLC determinations were similarly made using Merck NH 2 F 254S precoated glass plates (ϳ2 ؋ 5 cm, 5-m particle size, 0.2-mm layer thickness) with mixtures of acetonitrile, methanol, and water containing 0.1% diethylamine (v/v). Preexisting traces of carcinogenic nitrosamines were detected in some samples of diazeniumdiolates. The methods provide a more efficient means of characterizing the purity of diazeniumdiolate samples prepared for use in biomedical applications than older procedures which rely on differential absorbance measurements at 250 and 350 nm, respectively.