Gerding T K, Drenth B F, Van de Grampel V J, Niemeijer N R, De Zeeuw R A, Tepper P G, Horn A S
Department of Toxicology, State University, Groningen, The Netherlands.
J Chromatogr. 1989 Jan 27;487(1):125-34. doi: 10.1016/s0378-4347(00)83014-5.
This paper describes an enzymic derivatization procedure that allows accurate determination of very small amounts of enantiomeric impurities in the D-2 dopamine agonist 2-(N-propyl-N-2-thienylethylamino)-5-hydroxytetralin (N-0437). After pre-column glucuronidation of the individual enantiomers, two diastereoisomers were formed which were separated by reversed-phase high-performance liquid chromatography. An enantiomeric purity of 99.84% was calculated for the (-)-enantiomer, against 99.89% for the (+)-enantiomer. The assay was validated by spiking 1% of the (-)-enantiomer in the (+)-enantiomer. A high accuracy (error 4.5%) and precision (coefficient of variation 2.9%, n = 5) of the method were established.
本文描述了一种酶促衍生化程序，该程序可准确测定D-2多巴胺激动剂2-(N-丙基-N-2-噻吩基乙氨基)-5-羟基四氢萘(N-0437)中极少量的对映体杂质。在各对映体进行柱前葡萄糖醛酸化后，形成了两种非对映异构体，通过反相高效液相色谱法进行分离。计算得到(-)-对映体的对映体纯度为99.84%，而(+)-对映体为99.89%。通过在(+)-对映体中加入1%的(-)-对映体对该测定法进行了验证。该方法具有高准确度(误差4.5%)和精密度(变异系数2.9%，n = 5)。
