Ito T, Matsuki Y, Kurihara H, Nambara T
J Chromatogr. 1987 Jun 5;417(1):79-87. doi: 10.1016/0378-4347(87)80093-2.
A sensitive method for the determination of captopril in blood and urine by gas chromatography-mass spectrometry is described. In order to prevent oxidative degradation of captopril, its sulph-hydryl group was immediately protected by treatment with N-ethylmaleimide (NEM), and the resulting NEM adduct was then converted into the bis(pentafluorobenzyl) derivative. Derivatized captopril was separated on a 2% OV-1 column, exhibiting a single peak of the correct theoretical shape. The detection limit was estimated to be 100 pg by using S-benzylcaptopril as an internal standard. The blood level and urinary excretion of unchanged captopril orally administered to dogs were determined by the proposed method. In addition, epimerization of the proline moiety and formation of the sulphoxide or sulphone through the esterification step are also described.
描述了一种通过气相色谱-质谱法测定血液和尿液中卡托普利的灵敏方法。为防止卡托普利的氧化降解，其巯基通过用N-乙基马来酰亚胺（NEM）处理立即得到保护，然后将所得的NEM加合物转化为双（五氟苄基）衍生物。衍生化的卡托普利在2% OV-1柱上分离，呈现出具有正确理论形状的单峰。以S-苄基卡托普利为内标，检测限估计为100 pg。通过所提出的方法测定了口服给予犬的未变化卡托普利的血药浓度和尿排泄量。此外，还描述了脯氨酸部分的差向异构化以及通过酯化步骤形成亚砜或砜的情况。
