Hanna G M, Lau-Cam C A
Food and Drug Administration, New York Regional Laboratory, Brooklyn 11232.
J Assoc Off Anal Chem. 1989 Jul-Aug;72(4):556-8.
Use of proton nuclear magnetic resonance spectroscopy and the lanthanide shift reagent, Eu(hfc)3, resulted in a simple and reliable method for determination of the diastereomeric purity of trans-2-phenylcyclopropylamine sulfate (tranylcypromine sulfate). Eu(hfc)3 effectively simplified the complex overlapping pattern of the 5 non-equivalent phenyl protons to a virtually first order pattern. At a shift reagent to substrate molar ratio of 0.75, and a substrate concentration of 0.25M (as the free base) in CDCl3, the resonances for the cis- and trans-ortho-phenyl protons at 11.39 and 9.99 ppm, respectively, were sufficiently resolved to be of use in quantitative work. Analysis of synthetic diastereomeric mixtures of 2-phenylcyclopropylamine sulfate by the proposed method yielded results that were in close agreement with the expected values. The mean recovery (SD) of trans-diastereomer was 100.51% (0.40) (n = 6). Levels of less than 2% of cis-diastereomer were measurable in cis-trans mixtures.
使用质子核磁共振光谱法和镧系位移试剂Eu(hfc)3，得到了一种简单可靠的方法来测定反式-2-苯基环丙胺硫酸盐（反苯环丙胺硫酸盐）的非对映体纯度。Eu(hfc)3有效地将5个不等价苯基质子的复杂重叠图谱简化为几乎是一级图谱。在位移试剂与底物的摩尔比为0.75，且底物浓度为0.25M（以游离碱计）于CDCl3中的条件下，顺式和反式邻位苯基质子的共振峰分别在11.39和9.99 ppm处得到充分分辨，可用于定量分析。用所提出的方法分析2-苯基环丙胺硫酸盐的合成非对映体混合物，所得结果与预期值非常吻合。反式非对映体的平均回收率（标准差）为100.51%（0.40）（n = 6）。在顺反混合物中，可检测到的顺式非对映体含量低于2%。
