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本文建立了血浆中美托洛尔(Ⅰ)的直接手性分离方法。色谱条件采用Chiralcel OD分析柱(250×4.6 mm,id),RCSS硅胶预柱,流动相为异丙醇-正己烧-二乙胺(25:75:0.05,v/v),流速1.0 ml/min,荧光检测225 nm/295 nm。样品制备于每份0.5～1.0 ml血浆中加入100μl 1mol/L NaOH,涡旋10s,加正己烧3ml,振摇10min,离心(2000g,10min),水层于CO_2和甲醇混合液中冷冻,有机层于60℃挥去溶剂,残渣用50μl外标(S-烯丙洛尔)溶液(2μg/ml;溶剂为正己烷-异丙醇,5:1,v/v) 溶解,涡旋15s,进样
In this paper, a direct chiral separation method of metoprolol (Ⅰ) in plasma was established. Chromatography was performed on a Chiralcel OD analytical column (250 × 4.6 mm, id) using a RCSS silica gel column with a mobile phase of isopropanol-n-butylamine (25:75:.05, v / v) min, fluorescence detection 225 nm / 295 nm. Samples were prepared in each 0.5 ~ 1.0 ml of plasma by adding 100μl 1mol / L NaOH, vortexed 10s, plus 3ng Sinocrost, shaken 10min, centrifuged (2000g, 10min), the aqueous layer was CO_2 and methanol mixture frozen, organic The layers were evaporated at 60 ° C and the residue was dissolved in 50 μl of an external standard solution (2 μg / ml; solvent n-hexane-isopropanol, 5: 1, v / v) Injection