人血浆中乙胺碘呋酮的高效液相色谱法测定

应用改性甲醇(500ml甲醇中加入0.25 ml丁胺,混匀,继加1.0 ml 1:1冰醋酸为流动相,在YWG-CN(腈基键合相)柱上,以回苏灵(dimefline)为内标,对乙胺碘呋酮建立了适合于临床药理和临床化学应用的高效液相色谱测定法。本法简便、快速、灵敏、重现性好,流动相无需脱气并可循环使用。样品用乙醚提取,乙胺碘呋酮及回苏灵的平均回收率均大于97%。测定结果的变异系数,日内小于3.5%,日问小于5.0%。

DETERMINATION OF AMIODARONE IN HUMAN PLASMA BY HIGH PERFORMANCE LIQUID CHROMATOGRAPHY

A liquid chromatographic method has been developed for determination of amiodarone in human plasma using a chemically bonded eyano phase column (YWG -CN, 10μm)with dimefline as internal standard and modified methanol (0.25 ml of n-butylamine and 1.0 ml of 1:1 glacial acetic acid added to 500 ml of methanol) as mobile phase used in recycle mode. The procedure was as follows: Transfer 0.5ml of patient plasma into a 12ml of glass centrifuge tube, add 10μ1 of the internal standard (0.1μg/μ1) and 9ml of ethyl ether pre-treated with 0.2 M phosphate buffer (pH6.0) containing 0.1% sodium metabisulfite. Shake for 5 minutes and centrifuge for 5 minutes at 3000 rpm. Transfer the ethyl ether phase into another tube, add a few drops of chloroform saturated with concentrated hydrochloric acid and evaporate to dryness at 50℃. Reconstitute the residue with 50μ1 of mobile phase and inject 20μ1 into the chromatograph.The absolute recoveries of amiodarone and internal standard were found to be above 97% and the method was linear from 0.4 to 10μg/ml with a correlation coefficient of 0.998. The coefficient of variation was less than 3.5% for within day (n=8) and less than 5.0% for between day (n=8) respectively.