Chu Bao-Lin, Guo Bao-Yuan, Wang Zhihua, Lin Jin-Ming
State Key Laboratory of Chemical Resource Engineering, Beijing University of Chemical Technology, Beijing, China.
J Sep Sci. 2008 Dec;31(22):3911-20. doi: 10.1002/jssc.200800378.
A comparison between chiral cyclodextrin-modified microemulsion electrokinetic chromatography (CD-MEEKC) and cyclodextrin-modified micellar electrokinetic chromatography (CD-MEKC) for the enantiomeric separation of esbiothrin was carried out. For both methods, the separation conditions were optimized by varying CD types and concentration, running buffer pH and compositions, organic modifiers, and temperature. The optimal CD-MEEKC conditions were 0.8% n-heptane, 2.3% SDS, 6.6% n-butanol, 90.3% 10 mM sodium tetraborate containing 3% (w/v, the ratio of CD mass to microemulsion volume) methyl-beta-cyclodextrin, pH 10, 25 degrees C. The optimized CD-MEKC conditions were 3.3% SDS, 96.7% 10 mM sodium tetraborate containing 5% (w/v) beta-CD, pH 10, 25 degrees C. The difference in physicochemical properties of the buffer and CDs resulted in different optimal CD type. The competitive distribution between the microemulsion (or micelle) and chiral CD contributed to the chiral separation. Both methods provided excellent separation (R(s) approximately 3) with similar migration time (ca. 15 min). CD-MEEKC provided higher separation efficiencies (>300000) than CD-MEKC (>200000). The LODs for CD-MEEKC and CD-MEKC were 4.7 microg/mL and 3.2 microg/mL, respectively. The RSDs of migration time and peak area for CD-MEEKC were slightly higher than for CD-MEKC. Both the demonstrated CD-MEEKC and CD-MEKC methods provided high efficiencies, low LODs, and reproducible enantioseparations of esbiothrin.
对手性环糊精修饰的微乳液电动色谱法(CD - MEEKC)和环糊精修饰的胶束电动色谱法(CD - MEKC)分离乙虫腈对映体进行了比较。对于这两种方法,通过改变环糊精类型和浓度、运行缓冲液的pH值和组成、有机改性剂以及温度来优化分离条件。CD - MEEKC的最佳条件为:0.8%正庚烷、2.3%十二烷基硫酸钠(SDS)、6.6%正丁醇、90.3%含3%(w/v,环糊精质量与微乳液体积之比)甲基 - β - 环糊精的10 mM硼酸钠,pH值为10,25℃。优化后的CD - MEKC条件为:3.3% SDS、96.7%含5%(w/v)β - 环糊精的10 mM硼酸钠,pH值为10,25℃。缓冲液和环糊精物理化学性质的差异导致了最佳环糊精类型的不同。微乳液(或胶束)与手性环糊精之间的竞争分配促成了手性分离。两种方法都实现了出色的分离(Rs约为3),迁移时间相似(约15分钟)。CD - MEEKC的分离效率(>300000)高于CD - MEKC(>200000)。CD - MEEKC和CD - MEKC的检测限分别为4.7 μg/mL和3.2 μg/mL。CD - MEEKC迁移时间和峰面积的相对标准偏差略高于CD - MEKC。所展示的CD - MEEKC和CD - MEKC方法都提供了高效、低检测限且可重现的乙虫腈对映体分离。