Hanna G M, Lau-Cam C A
Food and Drug Administration, Department of Health and Human Services, New York Regional Laboratory, Brooklyn 11239-1593.
J Pharm Biomed Anal. 1989;7(8):919-28. doi: 10.1016/0731-7085(89)80016-0.
A simple, specific and reliable 1H-NMR spectroscopic method for the quantitative determination of the optical purity of indacrinone is described. After conversion of the S(+)- and R(-)-enantiomers to their methyl ester derivatives, they were coordinated with chiral europium(III) or praseodymium(III) shift reagents in CCl4/C2HCl3 (2:1). The optical purity was calculated from the relative intensities of the enantiomeric resonance signals for the protons of the methyl groups at position C(2) of the indanone ring. Mean +/- SD (n = 6) recoveries of S(+)-indacrinone from synthetic enantiomeric mixtures amounted to 99.75 +/- 0.63% when using europium(III) and 100.01 +/- 0.55% when using praseodymium(III).
描述了一种用于定量测定茚达立酮光学纯度的简单、特异且可靠的¹H-NMR光谱法。将S(+)-和R(-)-对映体转化为它们的甲酯衍生物后，使其在CCl₄/C₂HCl₃（2:1）中与手性铕(III)或镨(III)位移试剂配位。根据茚满酮环C(2)位甲基质子的对映体共振信号的相对强度计算光学纯度。当使用铕(III)时，从合成对映体混合物中回收S(+)-茚达立酮的平均回收率±标准差（n = 6）为99.75±0.63%，使用镨(III)时为100.01±0.55%。
