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Design, synthesis and evaluation of a series of alkylsiloxane-bonded stationary phases for expanded supercritical fluid chromatography separations
Fu, Qing1; Jiang, Dasen1; Xin, Huaxia1; Dai, Zhuoshun1; Cai, Jianfeng1; Ke, Yanxiong1; Jin, Yu1; Liang, Xinmiao1,2
Corresponding AuthorJin, Yu(Jiny@ecust.edu.cn)
KeywordSupercritical fluid chromatography Alkylsiloxane-bonded stationary phases Linear solvation energy relationship Selectivity Retention mechanism
Source PublicationJOURNAL OF CHROMATOGRAPHY A
2019-05-24
ISSN0021-9673
DOI10.1016/j.chroma.2019.01.069
Volume1593Pages:127-134
WOS SubjectBiochemical Research Methods ; Chemistry, Analytical
WOS Research AreaBiochemistry & Molecular Biology ; Chemistry
WOS KeywordREVERSED-PHASE ; MASS-SPECTROMETRY ; CLASSIFICATION ; RETENTION ; SELECTIVITY ; IMPROVE
AbstractSupercritical fluid chromatography (SFC) today represents an alternative technique in analytical chemistry due to its obvious benefits in kinetic performance and its complementarity to liquid chromatography. In this paper, a series of alkylsiloxane-bonded stationary phases were synthesized and evaluated to expand their SFC applications. Five kinds of non-endcapped C8 stationary phases (C8-1 to C8-5) with increasing bonding density were synthesized, and the carbon content was 3.91%, 6.07%, 7.97%, 8.65% and 9.10% respectively. Retention mechanism of the C8 phases in SFC in SFC was investigated by the use of a linear solvation energy relationship (LSER) model. Results underlined a close relationship between the bonding density of alkyl chain and the dispersion and polar interactions of the stationary phase. Complementary evaluation was studied based on the calculation of vector angle (theta), and the widest theta of 123 degrees was found between silica and C8 with the highest bonding density. Selective diversity also existed between the two C8 phases with the highest and lowest bonding densities. In addition, the effect of modifier on the SFC mechanism was investigated. Modifiers (methanol, ethanol, isopropanol and acetonitrile) had insignificant influence on the dispersion interaction but they mainly affected the hydrogen bonding interaction by changing the LSER parameters a and b. Finally, C8 and silica columns were applied for separation of eight amide alkaloids of Piper kadsura. Silica provided better retention but limited selectivity while C8 can distinguish alkaloids different in alkyl chain, double bond and cis-trans structure. This research further contributed to demonstrate the potential of alkylsiloxane-bonded stationary phase in improving selectivity of SFC. (C) 2019 Elsevier B.V. All rights reserved.
Language英语
WOS IDWOS:000466620100015
PublisherELSEVIER SCIENCE BV
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Document Type期刊论文
Identifierhttp://cas-ir.dicp.ac.cn/handle/321008/165525
Collection中国科学院大连化学物理研究所
Corresponding AuthorJin, Yu
Affiliation1.East China Univ Sci & Technol, Sch Pharm, Minist Educ, Engn Res Ctr Pharmaceut Proc Chem, Shanghai 200237, Peoples R China
2.Chinese Acad Sci, Dalian Inst Chem Phys, Key Lab Nat Med, Key Lab Separat Sci Analyt Chem, Dalian 116023, Liaoning, Peoples R China
Recommended Citation
GB/T 7714
Fu, Qing,Jiang, Dasen,Xin, Huaxia,et al. Design, synthesis and evaluation of a series of alkylsiloxane-bonded stationary phases for expanded supercritical fluid chromatography separations[J]. JOURNAL OF CHROMATOGRAPHY A,2019,1593:127-134.
APA Fu, Qing.,Jiang, Dasen.,Xin, Huaxia.,Dai, Zhuoshun.,Cai, Jianfeng.,...&Liang, Xinmiao.(2019).Design, synthesis and evaluation of a series of alkylsiloxane-bonded stationary phases for expanded supercritical fluid chromatography separations.JOURNAL OF CHROMATOGRAPHY A,1593,127-134.
MLA Fu, Qing,et al."Design, synthesis and evaluation of a series of alkylsiloxane-bonded stationary phases for expanded supercritical fluid chromatography separations".JOURNAL OF CHROMATOGRAPHY A 1593(2019):127-134.
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