## Abstract Heptafluorobutyl chloroformate (HFBCF), a recently introduced derivatization reagent, was examined in enantioseparation of amino acids (AAs) by GC. Twenty proteinogenic AAs, plus ornithine, cystine and 4‐fluorophenylalanine (internal standard) were treated with the reagent and separatio
Relationship between GC retention and physicochemical parameters of amino acids on chirasil-val
✍ Scribed by Rácz, Zsuzsanna ;Cserháti, Tibor
- Publisher
- John Wiley and Sons
- Year
- 1990
- Tongue
- English
- Weight
- 189 KB
- Volume
- 13
- Category
- Article
- ISSN
- 0935-6304
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✦ Synopsis
decomposition was observed. The reaction completeness was checked with mobile phase B because in mobile phase A the promethazine peak, R t 3.10 min, did not separate from other peaks. A baseline separation was obtained for the diastereoisomers with mobile phase A (Figure 3) with a resolution of 2.0. Mobile phase B gave a similar separation but with longer retention times (Figure 2). The chromatographic position of the individual enantiomers was checked with the pure promethazine enantiomers. The latter were obtained by crystallization [l]. The enantiomeric purity of the promethazine enantiomers thus obtained was verified with a Chiral a-AGP stationary phase (ChromTech, Stockholm, Sweden). After derivatization with (-)-menthy1 chloroformate the (-)-prornethazine derivative eluted before the (+) derivative in the RP-HPLC system.
So far, derivatizations with (-)-menthy1 chloroformate have been described for secondary amines [2, 31 and for one tertiary amine, namely encainide [4]. The procedure described here is quicker and easier and has the advantage that a RP-HPLC column can be used, 121 131 141 Short Communications which facilitates the handling of biological samples. Since many relevant drugs are secondary or tertiary amines, it may be expected that this approach can be useful for other substances as well. The procedure described is fast, reproducible, and apparently insensitive to side reactions or interfering products.
References
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