Urmös I, Benkö S M, Klebovich I
Department of Pharmacokinetics, EGIS Pharmaceuticals Ltd., Budapest, Hungary.
J Chromatogr. 1993 Jul 23;617(1):168-72. doi: 10.1016/0378-4347(93)80438-a.
A validated, sensitive and rapid high-performance high-performance liquid chromatographic method has been developed for the analysis of both cis and trans isomers of clomiphene in human plasma. The method involves a new off-line pre-column solid-phase extraction for sample preparation of clomiphene from human plasma in the presence of an internal standard. Analysis was performed by isocratic elution on a LiChrospher 100 RP-18 5-microns column using on-line post-column photochemical derivatization, with fluorescence detection at 247 nm (excitation) and 378 nm (emission). The limit of quantitation was 0.75 ng/ml for the cis isomer and 1.25 ng/ml for the trans isomer. The precision and accuracy of method were between good laboratory practice (GLP) required limits.
已开发出一种经过验证的、灵敏且快速的高效液相色谱法,用于分析人血浆中克罗米酚的顺式和反式异构体。该方法涉及一种新的离线柱前固相萃取,用于在存在内标的情况下从人血浆中制备克罗米酚样品。采用等度洗脱,在LiChrospher 100 RP - 18 5微米柱上进行分析,使用在线柱后光化学衍生化,在247 nm(激发)和378 nm(发射)处进行荧光检测。顺式异构体的定量限为0.75 ng/ml,反式异构体的定量限为1.25 ng/ml。该方法的精密度和准确度在良好实验室规范(GLP)要求的限度范围内。