Suzuki A, Takagaki S, Suzuki H, Noda K
Department of Pharmacokinetics and Drug Metabolism, Fujisawa Pharmaceutical Co., Ltd., Osaka, Japan.
J Chromatogr. 1993 Aug 11;617(2):279-84. doi: 10.1016/0378-4347(93)80499-t.
An enantioselective liquid chromatographic assay for the determinations of the R,R- and S,S-enantiomers of vamicamide, a potent anticholinergic drug, in human serum and urine is described. Racemic vamicamide and internal standard were purified from biological fluids using a two-step extraction procedure involving diethyl ether and 0.1% phosphoric acid. The overall recoveries of racemic vamicamide and internal standard were greater than 80%. The purified samples were measured by high-performance liquid chromatography on a Chiral-AGP column with ultraviolet absorbance detection at 260 nm. The standard curves for the analytes were linear from 10 to 200 ng/ml in serum and from 0.25 to 50 micrograms/ml in urine. The quantification limit of both enantiomers was 10 ng/ml for serum and 250 ng/ml for urine. Both intra-day and inter-day accuracy and precision data showed good reproducibility of the method. The assay has been applied for the analysis of vamicamide enantiomers in serum and urine samples from a healthy volunteer.
本文描述了一种对映体选择性液相色谱法，用于测定强效抗胆碱能药物瓦米卡胺的R,R-和S,S-对映体在人血清和尿液中的含量。外消旋瓦米卡胺和内标物通过两步萃取法从生物流体中纯化，该方法涉及使用乙醚和0.1%磷酸。外消旋瓦米卡胺和内标物的总回收率大于80%。纯化后的样品通过高效液相色谱法在Chiral-AGP柱上进行测定，在260nm处采用紫外吸收检测。分析物在血清中的标准曲线在10至200 ng/ml范围内呈线性，在尿液中的标准曲线在0.25至50μg/ml范围内呈线性。两种对映体在血清中的定量限为10 ng/ml，在尿液中的定量限为250 ng/ml。日内和日间的准确度和精密度数据均表明该方法具有良好的重现性。该测定法已应用于分析一名健康志愿者的血清和尿液样本中的瓦米卡胺对映体。
