Hanna G M, Lau-Cam C A
Food and Drug Administration, Department of Health and Human Services, New York Regional Laboratory, Brooklyn 11232-1593.
Pharm Res. 1990 Jul;7(7):726-9. doi: 10.1023/a:1015815605583.
A 1H-NMR spectroscopic method for the determination of the optical purity of threo-methylphenidate hydrochloride is presented. Complexation of the free-base form of the substrate with a chiral Eu(III) shift reagent resulted in two distinct enantiomeric ester methyl proton signals of utility for quantitative work. The accuracy of the method was validated by analyzing six synthetic mixtures of various proportions of (+)- and (-)-threo-methylphenidate. In addition to yielding assay results that were in close agreement with the known weights of each enantiomer in the mixture, and a mean recovery of the (-)-threo-enantiomer of better than 99.0%, the proposed method was capable of accurately measuring as little as 2% of one enantiomer in the presence of the other.
本文介绍了一种用于测定盐酸苏式哌醋甲酯光学纯度的1H-NMR光谱法。底物的游离碱形式与手性铕（III）位移试剂络合，产生两个不同的对映体酯甲基质子信号，可用于定量分析。通过分析六种不同比例的（+）-和（-）-苏式哌醋甲酯的合成混合物，验证了该方法的准确性。除了得到的测定结果与混合物中各对映体的已知重量密切一致，且（-）-苏式对映体的平均回收率优于99.0%外，该方法还能够在存在另一种对映体的情况下准确测量低至2%的一种对映体。
