Han K S, Woo S J, Koo C H, Lee M G
College of Pharmacy, Seoul National University, South Korea.
J Chromatogr B Biomed Sci Appl. 1998 Jun 12;710(1-2):239-42. doi: 10.1016/s0378-4347(98)00097-8.
A high-performance liquid chromatographic method was developed for the determination of a chemoprotective agent, 2-(allylthio)pyrazine (I), in human plasma and urine, and in rat blood and tissue homogenate using diazepam as an internal standard. The sample preparation was simple; 2.5 volumes of acetonitrile were added to the biological sample to deproteinize it. A 50-100 microl aliquot of the supernatant was injected onto a C18 reversed-phase column. The mobile phase employed was acetonitrile-water (55:45, v/v), and it was run at a flow-rate of 1.5 ml/min. The column effluent was monitored using an ultraviolet detector at 330 nm. The retention times for I and the internal standard were 4.0 and 5.1 min, respectively. The detection limits of I in human plasma and urine, and in rat tissue homogenate (including blood) were 20, 20 and 50 ng/ml, respectively. The coefficients of variation of the assay (within-day and between-day) were generally low (below 6.1%) in a concentration range from 0.02 to 10 microg/ml for human plasma and urine, and for rat tissue homogenate. No interferences from endogenous substances were found.
建立了一种高效液相色谱法，以地西泮为内标，用于测定人血浆、尿液以及大鼠血液和组织匀浆中的化学保护剂2-(烯丙硫基)吡嗪（I）。样品制备简单；向生物样品中加入2.5倍体积的乙腈使其脱蛋白。取50 - 100微升上清液注入C18反相柱。所用流动相为乙腈 - 水（55:45，v/v），流速为1.5毫升/分钟。使用紫外检测器在330纳米处监测柱流出物。I和内标的保留时间分别为4.0分钟和5.1分钟。I在人血浆、尿液以及大鼠组织匀浆（包括血液）中的检测限分别为20、20和50纳克/毫升。在人血浆、尿液以及大鼠组织匀浆浓度范围为0.02至10微克/毫升时，该测定法的变异系数（日内和日间）通常较低（低于6.1%）。未发现内源性物质的干扰。
