Evaluation of Separation Performance of Polydimethylsiloxane-Matrixed Chromatography by NMR

doi:10.11938/cjmr20150312

Chinese Journal of Magnetic Resonance ›› 2015, Vol. 32 ›› Issue (3): 511-517.doi: 10.11938/cjmr20150312

Previous Articles Next Articles

Evaluation of Separation Performance of Polydimethylsiloxane-Matrixed Chromatography by NMR

WU Rui¹，BAI Zheng-wu^1*，YANG Ying²，HUANG Shao-hua^2*

1. School of Chemical and Environmental Engineering, Wuhan Institute of Technology, Wuhan 430073, China; 2. Key Laboratory of Biobased-materials, Qingdao Institute of Bioenergy and Bioprocess Technology, Chinese Academy of Sciences, Qingdao 266101, China

Received:2014-07-15 Revised:2015-07-20 Published:2015-09-05 Online:2015-09-05
About author:*Corresponding author: BAI Zheng-wu, Tel: +86-027-87194980, E-mail: zhengwu_bai@yahoo.com; HUANG Shao-hua, Tel: +86-0532-80662660, E-mail: huangsh@qibebt.ac.cn.
Supported by:
国家自然科学基金资助项目(21105108)

Abstract

Abstract:

Polydimethylsiloxane (PDMS) has been used as the virtual “stationary phase” (VSP) for chromatographic NMR. Its separation capability towards halogenated compounds was investigated. Diffusion coefficients of n-pentane, 1-bromopentane and 1,5-dibromopentane contained in a mixture were measured with high-resolution liquid-state diffusion-ordered NMR spectroscopy (DOSY). In the absence of PDMS, these diffusion coefficients were close, and as a result, the three components could not be separated. In contrast, the diffusion coefficients were markedly different from each other in the presence of PDMS, leading to excellent separation. In addition, the effects of sample temperature and solution viscosity on separation performance were also investigated. It was observed that separation performance improved as sample temperature rose; and reduced as solution viscosity increased.

Key words: polydimethylsiloxane, virtual stationary phase, chromatography NMR, DOSY, separation

CLC Number:

O482.53

WU Rui1，BAI Zheng-wu1*，YANG Ying2，HUANG Shao-hua2*. Evaluation of Separation Performance of Polydimethylsiloxane-Matrixed Chromatography by NMR[J]. Chinese Journal of Magnetic Resonance, 2015, 32(3): 511-517.

References

[1] Morris K F, Stilbs P, Johnson C S. Analysis of mixtures based on molecular-size and hydrophobicity by means of diffusion ordered 2D NMR[J]. Anal Chem, 1994, 66(2): 211－215.

[2] Carrara C, Lopez C, Caldarelli S. Chromatographic-nuclear magnetic resonance can provide a prediction of high-pressure liquid chromatography shape selectivity tests[J]. J Chromatogr A, 2012, 1 257: 204－207.

[3] Carrara C, Caldarelli S. Relative average mass transport properties of mixture components in the presence of a porous silica gel depend on the solution/solid phase ratio[J]. J Phys Chem C, 2012, 116(37): 20 030－20 034.

[4] Tian Yuan(田园), Tang Hui-ru(唐惠儒). Identification and structural determination of saccharides in rat feces(大鼠粪样中几种糖类物质的结构确定)[J]. Chinese J Magn Reson(波谱学杂志), 2012, 29(3): 361－371.

[5] Zhao Bin(赵兵), Li Yi-lei(李艺蕾), Liu Hong-min(刘宏民), et al. An NMR study of capsaicin/β-cyclodextrin complex(辣椒碱与β-环糊精包合物的核磁共振研究)[J]. Chinese J Magn Reson(波谱学杂志) , 2013, 30(4): 576－584.

[6] Novoa-Carballal R, Fernandez-Megia E, Jimenez C, et al. NMR methods for unravelling the spectra of complex mixtures[J]. Nat Prod Rep, 2011, 28(1): 78－98.

[7] Caldarelli S. Chromatographic NMR: a tool for the analysis of mixtures of small molecules[J]. Magn Reson Chem, 2007, 45: S48－S55.

[8] Price K E, Lucas L H, Larive C K. Analytical applications of NMR diffusion measurements[J]. Anal Bioanal Chem, 2004, 378: 1 405－1 407.

[9] Johnson C S. Diffusion ordered nuclear magnetic resonance spectroscopy: principles and applications[J]. Prog Nucl Magn Reson Spectrosc, 1999, 34: 203－256.

[10] Huang S, Wu R, Bai Z, et al. Evaluation of the separation performance of polyvinylpyrrolidoneas a virtual stationary phase for chromatographic NMR[J]. Magn Reson Chem, 2014, 52: 486－490.

[11] Viel S, Ziarelli F, Caldarelli S. Enhanced diffusion-edited NMR spectroscopy of mixtures using chromatographicstationary phases[J]. Proc Natl Acad Sci USA, 2003, 100(17): 9 696－9 698.

[12] Hoffman R E, Arzuan H, Pemberton C, et al. High-resolution NMR “chromatography” using a liquids spectrometer[J]. J Magn Reson, 2008, 194(2): 295－299.

[13] Reddy G N M, Ballesteros-Garrido R, Lacour J, et al. Determination of labile chiral supramolecular ion pairs by chromatographic NMR spectroscopy[J]. Angew Chem Int Ed, 2013, 52(11): 3 255－3 258.

[14] Kavakka J S, Kilpelainen I, Heikkinen S. General chromatographic NMR method in liquid state for synthetic chemistry: Polyvinylpyrrolidone assisted DOSY experiments[J]. Org Lett, 2009, 11(6): 1 349－1 352.

[15] Kavakka J S, Parviainen V, Wahala K, et al. Enhanced chromatographic NMR with polyethyleneglycol. A novel resolving agent for diffusion ordered spectroscopy[J]. Magn Reson Chem, 2010, 48: 777－781.

[16] Joyce R E, Day I J. Chromatographic NMR with size exclusion chromatography stationary phases[J]. J Magn Reson, 2012, 220: 1－7.

[17] Huang S, Gao J, Wu R, et al. Polydimethylsiloxane: A general matrix for high-performance chromatographic NMR separation[J]. Angew Chem Int Ed, 2014, 53: 11 592－11 595.

Evaluation of Separation Performance of Polydimethylsiloxane-Matrixed Chromatography by NMR

PDF (PC)

Knowledge

Abstract

Cite this article

share this article

References

Related Articles 15

Recommended Articles

Metrics

Comments

[1]	LIU Ying, YUAN Binhua, ZHANG Haowei. Design of a Portable Magnetic Resonance Multi-source RF Pulse Generator [J]. Chinese Journal of Magnetic Resonance, 2025, 42(3): 285-298.
[2]	JIANG Chaochao, YAO Shouquan, XU Juncheng, JIANG Yu. Design of the Broadband Magnetic Resonance Microcoil [J]. Chinese Journal of Magnetic Resonance, 2025, 42(3): 299-307.
[3]	SHU Wei. Diagnostic Efficacy Comparison of B-scan Ultrasonography and MRI in Fetal Skeletal Abnormalities [J]. Chinese Journal of Magnetic Resonance, 2025, 42(3): 265-274.
[4]	SUI Meiju, ZHANG Lei, WANG Ruifang, LUO Yingying, LI Sha, QIU Maosong, XU Qiuyi, CHEN Daiqin, CHEN Shizhen, ZHOU Xin. MRI-traceable Nanoenzyme for Cascade Catalysis-enhanced Immunotherapy [J]. Chinese Journal of Magnetic Resonance, 2025, 42(3): 231-248.
[5]	KOU Xinhui, ZHANG Yubing. Study on the Enantiomeric Recognition of Chiral Ureas Containing Amino Acid Units [J]. Chinese Journal of Magnetic Resonance, 2025, 42(3): 221-230.
[6]	MA Yingxue, ZHAO Yanqiang, YANG Xiaodong, JIANG Bin, TAO Cheng. Opportunities and Challenges of High-field and Ultra-high-field Magnetic Resonance Imaging in China [J]. Chinese Journal of Magnetic Resonance, 2025, 42(3): 334-344.
[7]	LI Keyan, CHENG Xin, CHEN Junfei, CAO Li, HUANG Zhen, LIU Chaoyang. Development of Low-noise Preamplifier for Low-field NMR [J]. Chinese Journal of Magnetic Resonance, 2025, 42(3): 321-333.
[8]	TANG Shihao, YANG Jinyu, XU Yajie, WANG Ya, PENG Bowen, GAO Yuhao, YANG Xiaodong. A Design of Circularly Polarized Coil for Low-field Nuclear Magnetic Resonance Spectrometers [J]. Chinese Journal of Magnetic Resonance, 2025, 42(3): 308-320.
[9]	HE Fengcheng, LI Mingdao, LV Xinglong, YAO Shouquan, JIANG Yu. Software Design of the Handheld NMR Spectrometer Console [J]. Chinese Journal of Magnetic Resonance, 0, (): 0-0.
[10]	. Structural Identification and Complete NMR Spectral Assignments of 4-Isopropoxy-1-(trifluoroacetyl)naphthalene [J]. Chinese Journal of Magnetic Resonance, 0, (): 0-0.
[11]	CHEN Bo, LIU Quan, MA Lei, CHEN Shunian, JIA Yaqi, ZHU Bin, GUO Junwang. Simulink-based Simulation Study of Continuous Wave Electron Paramagnetic Resonance Signal Processing and Detection [J]. Chinese Journal of Magnetic Resonance, 2025, 42(2): 174-183.
[12]	GU Jiajia, WANG Yuanjun. Hybrid Attention and Multiscale Module for Alzheimer's Disease Classification [J]. Chinese Journal of Magnetic Resonance, 2025, 42(2): 103-116.
[13]	ZUO Bingyu, SHI Lili, SONG Jia, ZHAO Yang, LI Qian. Application of Estrogen and Tumor Markers Combined with DCE-MRI in Diagnosis and Clinical Staging of Cervical Cancer [J]. Chinese Journal of Magnetic Resonance, 2025, 42(2): 164-173.
[14]	MENG Jingxin, WANG Yuanjun. Research Progress on Tractography of Superficial White Matter Based on Diffusion Magnetic Resonance Imaging [J]. Chinese Journal of Magnetic Resonance, 2025, 42(2): 205-220.
[15]	CHEN Jingcong, RAN Fengwei, ZHANG Haowei, LIU Ying. Optimization Methodology for Meningioma and Acoustic Neuroma Detection Model Based on DCGAN [J]. Chinese Journal of Magnetic Resonance, 2025, 42(2): 117-129.