Simultaneous Enantioseparation and Tandem UV-MS Detection of Eight -Blockers in Micellar Electrokinetic Chromatograph
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- 作者：Cevdet Akbay ; Syed A. A. Rizvi ; and Shahab A. Shamsi
- 刊名：Analytical Chemistry
- 出版年：2005
- 出版时间：March 15, 2005
- 年：2005
- 卷：77
- 期：6
- 页码：1672 - 1683
- 全文大小：739K
- 年卷期：v.77,no.6(March 15, 2005)
- ISSN：1520-6882
文摘
The feasibility of using a new and more versatile polymericchiral surfactant, i.e., poly(sodium N-undecenoxycarbonyl-L-leucinate (poly-L-SUCL) is investigated for simultaneous enantioseparation and detection of eightstructurally similar 
-blockers with tandem UV and MSdetection. Three optimization approaches, i.e., directinfusion-MS, capillary zone electrophoresis-MS, and chiralmicellar electrokinetic chromatography-mass spectrometry (CMEKC-MS), were investigated to optimize sheathliquid parameters, spray chamber parameters, and CMEKCseparation parameters for maximum sensitivity and chiralresolution. Compared to unpolymerized micelle of L-SUCL, the use of micelle polymer (i.e., poly-L-SUCL)provided significantly higher separation efficiency, lowerseparation current, and higher detection sensitivity forCMEKC-ESI-MS of -blockers. It was also observed that,unlike monomeric L-SUCL, polymeric L-SUCL providedenantioseparation of all -blockers even at the lowestsurfactant concentration (i.e., 5 mM poly-L-SUCL). Underoptimum CMEKC and ESI-MS conditions (15 mM poly-L-SUCL, 25 mM each of NH4OAc and TEA (pH 8.0); 80%(v/v) methanol sheath liquid containing 40 mM NH4OAc(pH 8.0); sheath liquid flow rate, 5.0 
L/min; drying gasflow rate, 5 L/min; drying gas temperature, 200 
C;nebulizing pressure, 6 psi (0.414 bar); capillary voltage,+2.5 kV; fragmentor voltage, 85 V), baseline enantioseparation of eight -blockers was achieved by tandem UV (in~30 min) and MS (in ~60 min) detection. Calibrationcurves for all -blockers were linear in the range of 0.01-0.6 mM for both CMEKC-UV and CMEKC-MS methods,but the later method provided better concentration limitof detection with similar RSD for migration time and peakareas. The CMEKC-ESI-MS method appears suitable foruse as a routine procedure for high-throughput separationof -blockers with high sensitivity.
-blockers with tandem UV and MSdetection. Three optimization approaches, i.e., directinfusion-MS, capillary zone electrophoresis-MS, and chiralmicellar electrokinetic chromatography-mass spectrometry (CMEKC-MS), were investigated to optimize sheathliquid parameters, spray chamber parameters, and CMEKCseparation parameters for maximum sensitivity and chiralresolution. Compared to unpolymerized micelle of L-SUCL, the use of micelle polymer (i.e., poly-L-SUCL)provided significantly higher separation efficiency, lowerseparation current, and higher detection sensitivity forCMEKC-ESI-MS of -blockers. It was also observed that,unlike monomeric L-SUCL, polymeric L-SUCL providedenantioseparation of all -blockers even at the lowestsurfactant concentration (i.e., 5 mM poly-L-SUCL). Underoptimum CMEKC and ESI-MS conditions (15 mM poly-L-SUCL, 25 mM each of NH4OAc and TEA (pH 8.0); 80%(v/v) methanol sheath liquid containing 40 mM NH4OAc(pH 8.0); sheath liquid flow rate, 5.0 L/min; drying gasflow rate, 5 L/min; drying gas temperature, 200 C;nebulizing pressure, 6 psi (0.414 bar); capillary voltage,+2.5 kV; fragmentor voltage, 85 V), baseline enantioseparation of eight -blockers was achieved by tandem UV (in~30 min) and MS (in ~60 min) detection. Calibrationcurves for all -blockers were linear in the range of 0.01-0.6 mM for both CMEKC-UV and CMEKC-MS methods,but the later method provided better concentration limitof detection with similar RSD for migration time and peakareas. The CMEKC-ESI-MS method appears suitable foruse as a routine procedure for high-throughput separationof -blockers with high sensitivity.