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HPLC测定血浆中尼美舒利浓度
Determination of nimesulide in plasma by HPLC
【摘要】 目的:建立测定血浆中尼美舒利(Nim)的反相高效液相色谱法。方法:血浆样品用甲醇沉淀蛋白,经酸化后加甲苯提取,氮气挥干,加流动相溶解进样。以YWGC18柱,甲醇0.05mol·L-1磷酸二氢钾(55∶45)为流动相,pH5.02,甲苯磺丁脲为内标,在波长230nm处检测。结果:在0.26μg·ml-1~10.8μg·ml-1浓度范围内,峰面积比与浓度呈良好线性关系,r=0.9995。最低检测限为0.2μg·ml-1,方法重现性好,方法回收率为86.0%~92.2%,萃取回收率为72.2%~88.4%。结论:用本方法测定8例单剂量po100mgNim的血药浓度,结果满意。
【Abstract】 OBJECTIVE: To determine the concentration of nimesulide in human plasma. METHOD: After addition of the internal standard (IS; tolbutamide), 0.5 ml of methanol and 0.3 ml of hydrochloric acid (1 mol·L-1) were added to 0.5 ml plasma. The nimesulide was extracted into 2 ml of toluene. The organic layer was evaporated to dryness under a stream of nitrogen, and the residue redissovled in 150 μl of mobile phase for HPLC injection. The drug and IS were chromatographed on C18 column with a mobile phase consisting of 0.05 mol·L-1 potassium dihydrogen phosphate solution (pH 5.02): methanol (55∶45) and detected at 230 nm. Chromatography was carried out at a flowrate of 1.0 ml·min-1 at room temperature (20 ℃). RESULTS: A better linearity was obtained from 0.256 5 μg to 10.78 μg of nimesulide per ml for plasma with a good correlation coefficient (r=0.999 58, n=8). The mininum detectable concentration was 0.2 μg·ml-1 for plasma. CONCLUSION: Drug concentration in plasma was determined by HPLC method following a single oral dose of 100 mg was given to 8 adult male volunteers. The procedure is presently being used in case work.
- 【文献出处】 中国药学杂志 ,CHINESE PHARMACEUTICAL JOURNAL , 编辑部邮箱 ,1998年05期
- 【分类号】R927.2
- 【被引频次】7
- 【下载频次】58