Hüttmann A, Mross K, Hossfeld D K
Department of Medicine, University Hospital Eppendorf, Hamburg, Germany.
J Chromatogr. 1993 Oct 29;620(2):233-8. doi: 10.1016/0378-4347(93)80009-s.
A high-performance liquid chromatographic method has been developed for the determination of the new podophyllotoxin derivative NK 611 in plasma samples. A solid-liquid extraction procedure with C18 extraction columns was used for extraction of plasma samples containing NK 611. The adsorbed NK 611 was eluted from the extraction columns with methanol-acetonitrile (50:50, v/v). The elution liquid was injected into a reversed-phase system consisting of a Chrompack C18 column. The mobile phase was acetonitrile-20 mM phosphate buffer, pH 7 (30:70, v/v). The UV detection mode allows sensitive determination of NK 611 in plasma within phase I trials. The limit of detection was 10 ng/ml, the limit of quantitation 35 ng/ml (for 1 ml of extracted plasma and 20-microliters injection volume). The calibration curve is linear within the concentration range 100-1000 ng/ml. The recovery of NK 611 from spiked plasma samples was approximately 80%.
已开发出一种高效液相色谱法，用于测定血浆样本中的新鬼臼毒素衍生物NK 611。采用C18萃取柱的固液萃取程序来萃取含NK 611的血浆样本。吸附在萃取柱上的NK 611用甲醇 - 乙腈（50:50，v/v）从萃取柱上洗脱下来。洗脱液注入由Chrompack C18柱组成的反相系统中。流动相为乙腈 - 20 mM磷酸盐缓冲液，pH 7（30:70，v/v）。紫外检测模式可在I期试验中灵敏地测定血浆中的NK 611。检测限为10 ng/ml，定量限为35 ng/ml（对于1 ml萃取血浆和20微升进样体积）。校准曲线在100 - 1000 ng/ml浓度范围内呈线性。从加标血浆样本中回收NK 611的回收率约为80%。
