Alembik M C, Wainer I W
U.S. Food and Drug Administration, Division of Drug Chemistry, Washington, DC 20204.
J Assoc Off Anal Chem. 1988 May-Jun;71(3):530-3.
A rapid, accurate method for separating and determining the enantiomeric composition of amphetamine bulk drug and commercial preparations was developed and subjected to collaborative study. Amide derivatives of the amphetamine enantiomers are formed by using achiral 2-naphthoyl chloride. The resulting enantiomeric amides are then chromatographed on a commercially available chiral stationary phase with hexane-isopropyl alcohol-acetonitrile (97 + 3 + 0.5) mobile phase, with detection at 254 nm. Seven collaborators received bulk drug and commercial samples of amphetamine. The collaborators and authors determined the mean percent l- and d-amphetamine from 2 injections of each sample. The method can detect the presence of as little as 0.5% of the l-enantiomer in d-amphetamine, with reproducibility between laboratories of +/- 71.3%. The method has been adopted official first action for determination of the enantiomeric composition of amphetamine bulk drug and preparations.
开发了一种快速、准确的方法用于分离和测定苯丙胺原料药及市售制剂的对映体组成，并进行了协同研究。苯丙胺对映体的酰胺衍生物通过使用非手性的2-萘甲酰氯形成。然后将所得的对映体酰胺在市售的手性固定相上进行色谱分离，流动相为己烷-异丙醇-乙腈（97 + 3 + 0.5），检测波长为254 nm。七名合作者收到了苯丙胺原料药和市售样品。合作者和作者对每个样品进样2次，测定了左旋和右旋苯丙胺的平均百分比。该方法能够检测出右旋苯丙胺中低至0.5%的左旋对映体，实验室间的重现性为±71.3%。该方法已被官方首次采用，用于测定苯丙胺原料药和制剂的对映体组成。
