论文部分内容阅读
为了改善基线，提高分离度和精密度，对文献报道测定环孢菌素的ＨＰＬＣ法在血样处理、色谱柱和流动相等方面作了改进。酸碱萃取以水平振荡代替涡旋混合，使样品的酸萃取和碱洗涤完全；洗涤重组样用的正己烷改用色谱纯，洗涤分两次进行，以彻底消除干扰；将１５０ｍｍ×４．６ｍｍ（１０μｍ）柱改为２５０ｍｍ×４．６ｍｍ（５μｍ）柱，并将流动相中乙腈－甲醇－注射用水的比例由６∶１∶３改为７∶３∶３，以提高柱效而又不延长测定时间；严格控制柱温和流动相纯度使基线平稳。改进后，环孢菌素Ａ和Ｄ的基线完全分离，回收率变异由９．０％减小到６．３％以下。并用该法测定了大鼠和家兔的血药浓度
In order to improve the baseline and improve the resolution and precision, the HPLC method for the determination of cyclosporin in the literature has been improved in terms of blood sample processing, column and mobile phase. Acid-base extraction with horizontal oscillation instead of vortex mixing, so that the sample acid extraction and alkaline washing completely; washed with a sample of n-hexane instead chromatography pure, washed in two separate to completely eliminate interference; 150mm × 4.6mm (10μm) column to a 250mm × 4.6mm (5μm) column, and changing the ratio of acetonitrile-methanol-water for injection from 6: 1: 3 to 7: 3: 3 in the mobile phase to improve the efficiency without Extend the measurement time; strict control of the column temperature and the purity of the mobile phase to make the baseline stable. After the improvement, the baseline of cyclosporin A and D were completely separated, and the recovery variation decreased from 9.0% to below 6.3%. The method was used to determine the blood concentration in rats and rabbits