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以手性冠醚为胶束毛细管电泳手性分离选择剂,对吉米沙星对映体药物的在线富集分离进行了研究。考察了阳离子表面活性剂十二烷基三甲基溴化铵浓度、运行缓冲溶液中有机添加剂含量和进样方式对对映体的富集和分离度的影响。使用未涂层毛细管柱(37cm×51μm,有效柱长30cm),45mmol/LBis-Tris缓冲液+10mmol/L十二烷基三甲基溴化铵(DTAB)+1mmol/L手性冠醚+11%乙腈为运行缓冲溶液(pH=4.0),在紫外检测波长280nm、运行电压-10kV、电动进样条件下,对吉米沙星对映体进行在线推扫(sweeping)富集分离,在基线分离的前提下,富集倍数可达600~700倍。吉米沙星浓度为0.3μmol/L时,两对映体峰高的相对标准偏差<4.0%(n=7)。本方法为毛细管电泳在痕量对映体药物分析等方面的应用提供了新方法。
Chiral amphiphilic micellar capillary electrophoresis was used as chiral separation selective reagent to study the enantioseparation of gemifloxacin enantiomers on-line. The effects of cationic surfactant dodecyltrimethylammonium bromide concentration, organic additives in running buffer solution and injection mode on enantiomeric enrichment and resolution were investigated. Uncoated capillary column (37 cm × 51 μm, effective column length 30 cm), 45 mmol / L Tris-Tris buffer + 10 mmol / L dodecyltrimethylammonium bromide (DTAB) + 1 mmol / L chiral crown ether + The enantiomers of Gemifloxacin were collected by sweeping enrichment and separation under the condition of electrokinetic injection under the conditions of UV detection wavelength of 280 nm and operating voltage of 10 kV with 11% acetonitrile as running buffer (pH = 4.0) Under the premise of separation, enrichment fold up to 600 to 700 times. When the concentration of gemifloxacin was 0.3 μmol / L, the relative standard deviation of peak height of two enantiomers was less than 4.0% (n = 7). This method provides a new method for the capillary electrophoresis in the trace enantiomer drug analysis.