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Unimicro Technologies, Inc. unimicrotech

Unimicro Technologies, Inc. www.unimicrotech.com. 主要内容 加压毛细管电色谱技术简介 加压毛细管电色谱在实际复杂样品中的应用. 微型化驱动力. 便携式的要求 样品的贵重化和微量化 环境保护的需要 经济因素. CEC, CE & Micro-HPLC. 毛细管电色谱的优势 毛细管电泳与微径液相的结合  高分离效率，高选择性，高分辨率  二维分离机理 纳升级技术，微型化的优势 无色谱柱反压的影响，可采用小颗粒填料进行快速分离 可方便地与质谱连接.

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Unimicro Technologies, Inc. unimicrotech

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  1. Unimicro Technologies, Inc. www.unimicrotech.com

  2. 主要内容 • 加压毛细管电色谱技术简介 • 加压毛细管电色谱在实际复杂样品中的应用

  3. 微型化驱动力 • 便携式的要求 • 样品的贵重化和微量化 • 环境保护的需要 • 经济因素

  4. CEC, CE & Micro-HPLC

  5. 毛细管电色谱的优势 • 毛细管电泳与微径液相的结合  高分离效率，高选择性，高分辨率  二维分离机理 • 纳升级技术，微型化的优势 • 无色谱柱反压的影响，可采用小颗粒填料进行快速分离 • 可方便地与质谱连接

  6. <R&D Magazine> The future of Chromatography “HPLC is a mature technology. For now, HPLC is all about refinement rather than revolution.” “I think the revolution will come when we get a 10- to 100-fold improvement in separation efficiencies. We have already seen the edges of this with capillary electrochromatography (CEC) and its potential to deliver exceedingly high plate counts and efficiencies for the separations. I don’t know what technology will deliver that performance advantage but when it comes, everything will change.”

  7. 电动分离技术

  8. 高效分离:600,000 p/m Separation of 4 PAHs on 1.5mm non-porous ODS . Column: 100mm i.d. x 28cm packed length. Mobile phase: 70% CH3CN/30% 4mM sodium tetraborate (pH 9.1). Voltage: 20kV. Injection: 5kV/2s. Detection: LIF, ex: 257nm, em: 400nm. Sample: a) Fluoranthene, b) Benz[a]anthracene, c) Banzo[k]fluoranthene, and d) Benzo[ghi]perylene. Anal. Chem.70(22), 787, 1998, Dadoo. R.; Zare R..; Annex. D ; Yan, C.

  9. 毛细管电色谱快速分离 Column: 100mm i.d. x 6.5cm packed with 1.5mm non-porous ODS. Mobile phase: 70% CH3CN/30% 2mM TRIS (pH 9). Voltage: 28kV. Injection: 1kV/1s. Detection: LIF, ex: 257nm, em: 400nm. Anal. Chem., 70(22), 787, 1998, Dadoo. R.; Zare R..; Annex. D ; Yan, C.

  10. 毛细管电色谱分离14种爆炸物 Column: 75mm i.d. x 17cm packed with 1.5mm non-porous ODS. Mobile phase: 15% CH3OH/85% 10mM MES (pH 8.5). Voltage: 12kV. Injection: 1kV/1s. Detection: UV @ 254nm. Bailey, C.; Yan, C., Anal. Chem., 70(15), 3275, 1998

  11. 毛细管电色谱分离6种毒品 Lim; Zare; Bailey; Rakestraw; Yan, Electrophoresis, 21(4), 737, 2000

  12. 加压毛细管电色谱 简 介

  13. TriSepTM-2000GV CEC System

  14. TriSepTM-2010GV

  15. TriSepTM-2100

  16. 加压毛细管电色谱 vs. 毛细管电泳 • 可同时分离中性和离子型化合物 • 不需手性添加剂而进行手性分离 • 可实现二元溶剂梯度洗脱 • 连续进样过程中无需切断高压电场，保证分离色谱柱内电场和电渗流的稳定 • 采用阀进样，提高了分析的精度和准确度 • 可方便地与在线样品预处理系统相联 • 可实施实时、在线的样品分析

  17. 毛细管电泳系统

  18. 毛细管电泳进样方式 • 流体动力学 • 进样端加压 • 出口端减压 • 位差进样 • 电迁移进样

  19. 毛细管电泳进样过程 切断高压电源  将毛细管进口端移入样品瓶  进样  将毛细管进口端移入缓冲液瓶  开启高压电源  电泳分离 电平衡被打破 受外界条件影响 重新建立电平衡 样品污染

  20. 进样 毛细管电泳的瓶颈问题 • 进样精度差 • 样品和缓冲液间污染 • 电场不断被打断，分析精度差 • 很难实施在线连续分析 • 处理实际复杂样品的能力较弱

  21. 加压毛细管电色谱 vs. 毛细管电泳 • 可同时分离中性和离子型化合物 • 不需手性添加剂而进行手性分离 • 可实现二元溶剂梯度洗脱 • 连续进样过程中无需切断高压电场，保证分离色谱柱内电场和电渗流的稳定 • 采用阀进样，提高了分析的精度和准确度 • 可方便地与在线样品预处理系统相联 • 可实施实时、在线的样品分析

  22. 加压毛细管电色谱 vs. HPLC 分离效率 速度 分辨率 峰容量 重现性 微型化

  23. 超高速分离 线性流速5.5 mm/s Column：1.5 um Particle, 100 um 100 mm; Voltage: 30 kV; Pressure: 3500 psi; Linear velocity：5.5 mm/sec

  24. 加压毛细管电色谱 vs. 毛细管液相色谱 pCEC, -30 kV, Other conditions were the same as in capillary-LC capillary-LC

  25. 超高分辨率 Column：EP-100-10-1.5-C18 Pressure: 3000 psi; HV: 30 kV; UV：254 nm Sample: 1647c (16 polycyclic aromatic hydrocarbons) pCEC World Record! 16 PAHs were baseline separated in 6 minutes! 1647c: standard reference material

  26. 超高效分离 Column：EP-100-10-1.5-C18 Pressure: 1000 psi; HV: 5 kV; UV：254 nm Sample: 1647c (16 polycyclic aromatic hydrocarbons) Theoretical plates: 250,000 / m

  27. 超高峰容量 The average peak width was 2.5 seconds, giving a 1400/hr peak capacity.

  28. 超高重现性 中性化合物的分离 Retention time (RT) and peak area (PA) reproducibility %RSD for 10 replicates Column: 3 μm C18, 100μm  200 mm

  29. 超高重现性 离子型化合物的分离 Retention time (RT) and peak area (PA) reproducibility %RSD for 9 replicates Column: 5 μm C18, 150μm  300 mm

  30. 超高重现性 二元溶剂梯度洗脱 Retention time (RT) and peak area (PA) reproducibility %RSD for 5 replicates Column: 3 μm C18, 100μm  200 mm

  31. 微型化 HPLC vs. pCEC

  32. UPLC vs. pCEC

  33. UPLC vs. pCEC

  34. UPLC vs. pCEC

  35. 加压毛细管电色谱 在复杂样品中的应用

  36. 加压毛细管电色谱 柱技术

  37. 色 谱 柱

  38. Yan, Chao. US Patent. 5,453163, 1995

  39. Wei, W; Luo, G; Yan, C., Am. Lab., 30(1), 20C-20E, 1998

  40. Lelievre, F.; Yan, C.; Zare, R., J. Chromatogr., A, 723(1), 145, 1996

  41. 分子印记柱手性分离 pH effect From top: pH=7.5 pH=6.0 pH=5.0 pH=4.0 pH=3.2 J. Sep. Sci. 26, 1, 2003, W. Yan, R. Gao, C. Yan

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