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supercritical fluid chromatography and Its Application in Lipid Isomer Separation

Journal of Analysis and Testing 2017年第4期1卷 330-334页

作者： Shiyao Song Huwei Liu Yu Bai Beijing National Laboratory for Molecular Sciences Key Laboratory of Bioorganic Chemistry and Molecular Engineering of Ministry of EducationInstitute of Analytical ChemistryCollege of Chemistry and Molecular EngineeringPeking UniversityBeijing 100871China

supercritical fluid chromatography(SFC),which uses supercritical fluid with higher diffusivity and lower viscosity than liquid as its mobile phase,can provide fast,green,high-throughput and good performance methods for the analysis of complicated *** is an advantageous alternative for the separation of polar and nonpolar compounds,and even chiral *** an important constituent of living organisms,lipids and the related lipidomics researches have attracted dramatic attention during the past *** separation and identification of lipids and lipid isomers are of great significance and remain *** this mini-review,the principle of SFC and its applications in lipid isomer separation are summarized.

关键词： supercritical fluid chromatography Lipid Isomers Mass spectrometry

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Simultaneous enantioseparation and simulation studies of atenolol,metoprolol and propranolol on Chiralpak^■IG column using supercritical fluid chromatography

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Journal of Pharmaceutical Analysis 2021年第6期11卷 746-756页

作者： Pranav A.Pandya Priyanka A.Shah Pranav S.Shrivastav Department of Chemistry School of SciencesGujarat UniversityAhmedabad380009India

Enantioseparation of threeβ-blockers,i.e.,atenolol,metoprolol and propranolol,was studied on amylose tris(3-chloro-5-methylphenylcarbamate)immobilized chiral stationary phase using supercritical fluid chromatography(SFC).The effect of organic modifiers(methanol,isopropanol and their mixture),column temperature and back pressure on chiral separation ofβ-blockers was *** chromatographic separation with respect to resolution,retention,and analysis time was achieved using a mixture of CO_(2) and 0.1%isopropyl amine in isopropanol:methanol(50:50,V/V),in 75:25(V/V)*** the optimized conditions,the resolution factors(Rs)and separation factors(a)were greater than3.0 and 1.5,***,with increase in temperature(25-45℃)and pressure(100-150 bars)there was corresponding decrease in retention factors(k),a and ***,a reverse trend(a and Rs)was observed for atenolol with increase in *** thermodynamic data from van’t Hoff plots revealed that the enantioseparation was enthalpy driven for metoprolol and propranolol while entropy driven for *** understand the mechanism of chiral recognition and the elution behavior of the enantiomers,molecular docking studies were *** binding energies obtained from simulation studies were in good agreement with the elution order found experimentally and also with the free energy *** method was validated in the concentration range of 0.5-10μg/m L for all the *** limit of detection and limit of quantitation ranged from 0.126 to 0.137μg/m L and 0.376-0.414μg/m L,*** method was used successfully to analyze these drugs in pharmaceutical preparations.

关键词： Enantioseparation supercritical fluid chromatography β-blockers Chiralpak^(■)IG column Molecular docking Binding energy

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Chiral Separation of Ibuprofen by supercritical fluid chromatography

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Chinese Journal of Chemical Engineering 2005年第6期13卷 741-746页

作者： HAN Soonkoo ROW Kyungho Center for Advanced Bioseparation Technology and Department of Chemical Engineering Inha University253 Yonghyun-DongNam-KuIncheon 402-751South Korea

The separation method using chiral stationary phase （CSP） for the preparation of enantioselective compound was widely used. In this work, supercritical fluid chromatography（SFC） was proposed to resolve the chiral mixtures. To determine the optimum operating conditions for the chiral separation of the racemic ibuprofen, the retention factors and resolutions with the change in pressure, temperature and the content of IPA （%, by volume） in supercritical CO2 were investigated. Experiments showed that the retention factor decreased with the increase of pressure and decrease in temperature. The retention factor was also influenced by the content of IPA in mobile phase, as the content of IPA in the supercritical fluid increased, the retention factor decreased. The resolution of the enantiomers became worse with the increase of IPA in the supercritical fluid. Through optimizing the experimental conditions, a SFC procedure with 13MPa, 311.15K and 4% IPA in CO2 was obtained. The peak shape of the enantiomers was symmetric with supercritical fluid chromatography when compared to the asymmetric peak shape obtained by the conventional liquid chromatography. This work demonstrated that the developed supercritical fluid chromatography procedure was suitable for the chiral separation of ibuprofen enantiomers.

关键词： chiral separation ibuprofen retention factor resolution supercritical fluid chromatography

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Rapid Separation of Five Cyclosporin Analogs by supercritical fluid chromatography

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Journal of Analytical Sciences, Methods and Instrumentation 2016年第2期6卷 23-32页

作者： Yuefei Shao Chunlei Wang Atsu Apedo Oliver Mcconnell Bioanalytical and Discovery Analytical Sciences Research & Development Bristol-Myers Squibb Princeton New Jersey USA

Recently there has been a resurgence of interest in cyclic peptides due to their therapeutic advantages in terms of potency, permeability, proteolytic stability, and unique selectivity relative to traditional smaller drug molecules. Cyclosporin is a family of cyclic peptides widely used as autoimmune suppression agents. Cyclosporin analogs consist of eleven amino acids with the main difference lying at the side chain of its amino acid residues. In this study, a single step separation method was developed utilizing supercritical fluid chromatography (SFC) to resolve five naturally occurring cyclosporin analogs (Cyclosporin A, B, C, D, and H) on a bare silica-packed column. The optimized method involved use of ethanol-modified carbon dioxide as mobile phase on a bare silica column at 80 °C and UV detection at 220 nm. Although column temperature and back pressure generally had insignificant effect on SFC separation, it was found in our study that increasing temperature and pressure greatly improved peak shape and resolution.

关键词： Cyclic Peptide Cyclosporin supercritical fluid chromatography

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Overview of the Analytical Lifecycle of supercritical fluid chromatography Methods

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American Journal of Analytical Chemistry 2016年第1期7卷 75-91页

作者： Bertyl Andri Amandine Dispas Roland Djang’eing’a Marini Philippe Hubert Department of Pharmacy CIRM Laboratory of Analytical Chemistry University of Liege (ULg) Liege Belgium

In recent times, the overall interest over supercritical fluid chromatography (SFC) is truly growing within various domains but especially for pharmaceutical analysis. However, in the best of our knowledge modern SFC is not yet applied for drug quality control in the daily routine framework. Among the numerous reported SFC methods, none of them could be found to fully satisfy to all steps of the analytical method lifecycle. Thereby, the present contribution aims to provide an overview of the current and past achievements related to SFC techniques, with a targeted attention to this lifecycle and its successive steps. The included discussions were therefore structured accordingly and emphasizing the analytical method lifecycle in accord with the International Conference on Harmonisation (ICH). Recent and important scientific outputs in the field of analytical SFC, as well as instrumental evolution, qualification strategies, method development methodologies and discussions on the topic of method validation are reviewed.

关键词： supercritical fluid chromatography Ultra High Performance supercritical fluid chromatography Analytical Method Lifecycle Quality by Design

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Analysis of traditional chinese medicines by supercritical fluid chromatography with packed columns

Analysis of traditional chinese medicines by supercritical f...

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30th International Symposium on Capillary chromatography、4th GC×GC Symposium、16th National Symposium and Exhibition on chromatography,i.e. 1st Dalian International Symposium and Exhibition on chromatography

作者： Liang Gao Tingting Wang Jie Zhang Lihua Zhang~* Weibing Zhang Yukui Zhang National Chromatographic Research and Analysis Center Dalian Institute of Chemical Physics Chinese Academy of Sciences 457 Zhongshan Road Dalian 116023 China

＜正＞For supercritical fluid chromatography（SFC）,the mobile phase is generally of high diffusivity and low viscosity,which is achievable with the combination of a compressible fluid,usually carbon dioxide,and a normal liquid,such as *** with HPLC,SFC with packed columns is 5-10 times faster than. In addition,its separation mechanism is similar to normal-phase HPLC since the mobile phase is less polar than the stationary phase.

关键词： supercritical fluid chromatography packed column traditional Chinese medicines

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Separation of substituted phenylpiperazine derivatives with immobilized polysaccharide-based chiral stationary phases by supercritical and subcritical fluid chromatography

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Journal of Chinese Pharmaceutical Sciences 2013年第3期22卷 244-251页

作者：黄珺珺袁牧广州医学院药物研究中心广东广州510182

Six newly synthesized racemic 1-（substituted phenyl）-4-[3-（indole-4-yl-oxy）-2-hydroxypropyl]-piperazine 1-6 were successfully resolved by carbon dioxide supercritical fluid chromatography （SFC） on an analytical scale column packed with immobilized polysaccharide-based chiral stationary phases （CSPs）. We found that separation on the Chiralpak IA CSP was superior to the other two immobilized CSPs （Chiralpak IB and Chiralpak IC）, and isopropanol （IPA） was a superior modifier compared to the other five solvents including ethanol, methanol, tetrahydrofuran, acetonitrile and dichloromethane. The effects of organic modifier composition, back pressure, and column temperature for enantioseparation of all six compounds were studied. Of the physical parameters studied, modifier composition had the greatest impact on retention. Changing temperature generally had less impact on retention but produced the greatest selectivity changes. The optimum condition was found as follows： Chiralpak IA column, column temperature 35 ~C, back pressure 120 bar, 35% IPA containing 0.1% diethylamine （v/v） in mobile phase, flow rate of mobile phase 3.0 mL/min, UV detection 283 nm. Separation of all six racemic compounds was completed within 10 rain and excellent resolution was obtained. Thus, SFC was found to be the methodology of choice for resolving the enantiomers of this class of compounds.

关键词： supercritical fluid chromatography Immobilized polysaccharide-based chiral stationary phases Enantiomerresolution Phenylpiperazine derivatives

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