摘要
目的 建立反相高效液相色谱 紫外法测定血浆中沙丁胺醇浓度的方法。方法 采用UltraspherCyano分析柱 (2 5 0mm×4.6mm ,5 μm) ,乙腈 甲醇 0 .0 2 5mol·L- 1 磷酸铵缓冲液 (pH2 .8) (2∶0 .5∶97.5 )为流动相 ,吗啡作内标。样品经离子对萃取纯化后进样 ,在 2 2 4nm波长下检测 ,按内标法定量。结果 标准曲线在 0 .5～ 32 μg·L- 1 内有良好线性 ,最低检测浓度为 0 .3μg·L- 1 ,萃取回收率在 93%～ 99%之间 ,方法回收率在 98%～ 10 9%之间 ,日内RSD小于 5 % ,日间RSD小于 8%。结论 本法具有快速简便 ,灵敏准确等特点 ,已用于测定沙丁胺醇缓释制剂生物利用度样品 70 0余个 。
OBJECTIVE This paper established a high performance liquid chromatography for the determination of salbutamol (SBA) in human plasma using morphine as the internal standard.METHOD A variable wavelength UV detector and Ultraspher Cyano column (5 μm,250 mm×4.6 mm,Beckman)were used.To the plasma sample 1.0,0.5 ml phosphate buffer (2.0 mol·L -1 ,pH9.0) containing 0.4% diphenylboric acid 2 aminoethyl ester was added,then extracted with 4.0 ml chloroform containing 1% tetraoctylammonium bromide.The organic layer was removed and extracted again with 200 μl (0.08 mol·L -1 ) acetic acid.100 μl of the acid layer was injected onto the column .The mobile phase of acetonitrile methanol pH2.8,0.025 mol·L -1 phosphate buffer (2∶0.5∶97.5) was pumped at the rate of 1.0 ml·min -1 through the column.The detector at 0.002 AUFS was set at 224 nm.RESULTS The retention times for SBA and morphine were 7.0 min and 8.3 min,respectively.The standard curve was linear over the concentration range of 0.5 to 32 μg·L -1 .The detection limit in plasma was 0.3 μg·L -1 .Extraction recovery was 93%～99%;The method recovery was 98%～109%;with intra day RSD less than 5%;inter day RSD less than 8%.CONCLUSION This method was found to be simple,rapid,sensitive and accurate for the determination of SBA in human plasma.
出处
《中国药学杂志》
EI
CAS
CSCD
北大核心
2000年第7期475-477,共3页
Chinese Pharmaceutical Journal
