Peak deformations in preparative supercritical fluid chromatography due to co-solvent adsorption

Glenne, Emelie; Leek, Hanna; Klarqvist, Magnus; Samuelsson, Jörgen; Fornstedt, Torgny

doi:10.1016/j.chroma.2016.09.019

Cited by 18 publications

(12 citation statements)

References 49 publications

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“…In addition to differences between sample diluent and mobile phase, injection effects can also be engendered by the adsorption of the diluent itself onto the stationary phase. Several SFC studies revealed that the most commonly used sample diluents, such as methanol or acetonitrile, showed a significant retention on various types of stationary phases [50,[57][58][59]. This behaviour can lead to a competition between the analyte and the diluent to access the stationary phase, which in turn, can result in unusual peak shapes.…”

Section: Online Lc X Sfc: Overcoming Injection Effectsmentioning

confidence: 99%

“…As previously mentioned, common co-solvents like methanol or acetonitrile, can adsorb onto SFC stationary phases. In two subsequent papers, Glenne et al [57,58] showed that, when injecting high solute concentrations and volumes in preparative SFC, a significant retention of the organic co-solvent could also cause unexpected elution bands. These deformations were attributed to competition between the solute and solvent molecules for the stationary phase sites.…”

Section: Online Lc X Sfc: Overcoming Injection Effectsmentioning

confidence: 99%

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Opportunities and challenges of liquid chromatography coupled to supercritical fluid chromatography

Burlet-Parendel¹,

Faure²

2021

TrAC Trends in Analytical Chemistry

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Section: Online Lc X Sfc: Overcoming Injection Effectsmentioning

confidence: 99%

Section: Online Lc X Sfc: Overcoming Injection Effectsmentioning

confidence: 99%

Opportunities and challenges of liquid chromatography coupled to supercritical fluid chromatography

Burlet-Parendel¹,

Faure²

2021

TrAC Trends in Analytical Chemistry

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“…5−7 In these studies, we demonstrated that commonly used cosolvents adsorb to polar stationary phases, competing with the solute for available adsorption sites and hence affecting the solute retention and peak shape. 6,7 The temperature and pressure also influence the retention in SFC. 3,8,9 The solute's solubility increases with increasing density; 10 this will generally result in an reduction in the retention.…”

Section: ■ Introductionmentioning

confidence: 99%

Impact of Methanol Adsorption on the Robustness of Analytical Supercritical Fluid Chromatography in Transfer from SFC to UHPSFC

et al. 2020

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In supercritical fluid chromatography (SFC), the retention of a solute depends on the temperature, density, pressure, and cosolvent fraction. Here, we investigate how the adsorption of the cosolvent MeOH changes with pressure and temperature and how this affects the retention of several solutes. The lower the pressure, the stronger the MeOH adsorption to the stationary phase; in addition, at low pressure, perturbing the pressure results in significant changes in the amounts of MeOH adsorbed to the stationary phase. The robustness of the solute retention was lowest when operating the systems at low pressures, high temperatures, and low cosolvent fractions in the eluent. Here, we found a clear relationship between the sensitivity of MeOH adsorption to the stationary phase and the robustness of the separation system. Finally, we show that going from classical SFC to ultrahigh-performance SFC (UHPSFC), that is, separations conducted with much smaller packing diameters, results in retention factors that are more sensitive to fluctuations in the flow rate than with traditional SFC. The calculated density profiles indicate only a slight density drop over the traditional SFC column (3%, visualized as lighter → darker blue in the TOC), whereas the drop for the UHPSFC one was considerably larger (20%, visualized as dark red → light green in the TOC). The corresponding temperature drops were calculated to be 0.8 and 6.5 °C for the SFC and UHPSFC systems, respectively. These increased density and temperature drops are the underlying reasons for the decreased robustness of UHPSFC.

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“…In contrast, ultra‐performance convergence chromatography (UPC 2 ), which integrates supercritical fluid chromatography (SFC) and UHPLC technologies , exhibits a number of advantages over HPLC techniques, including reduced run times and improved resolutions, due to the use of a special compacted column containing sub‐1.7 μm particles . In addition, UPC 2 uses a mobile phase consisting of compressed or supercritical CO 2 in addition to a small amount of cosolvent . Supercritical CO 2 has a similar density and solvating power to a liquid, but also exhibits a low volatility and good diffusion properties, leading to low column pressures, rapid analyses, and lower mobile phase costs .…”

Section: Introductionmentioning

confidence: 99%

“…More specifically, the total contents of the four components present in the ten samples purchased from a herbal medicine market in South Korea ranged from 1.996 to 6.947 mg/g, while the corresponding values for the three samples purchased from China ranged from 1.950 to 5.187 mg/g. Interestingly, none of the four chromones were detected in five samples (samples 9,[17][18][19][20] from South Korea and two samples (samples 15 and 16) from China, thereby indicating differences in the quality of these purchased S. divaricata samples. These results were similar to those reported by Kim et al[3], who reported that a number of S. divaricata samples originating from South Korea contained none of the four chromones.…”

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confidence: 97%

Ultra‐performance convergence chromatography method for the determination of four chromones and quality control of Saposhnikovia divaricata (Turcz.) Schischk.

Kim

Choi

Lee

2018

J of Separation Science

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Ultra-performance convergence chromatography is an environmentally friendly analytical technique that employs dramatically reduced amounts of organic solvents compared to conventional chromatographic methods. In this study, a rapid, sensitive, and environmentally friendly method based on ultra-performance convergence chromatography was developed for the quantification of four major chromones present in the roots of Saposhnikovia divaricata (Turcz.) Schischk. Using this method, the analysis time was significantly shortened compared to conventional high-performance liquid chromatography techniques. In addition, the influence of cosolvent type, cosolvent ratio, column temperature, system pressure, and flow rate on the peak resolution was investigated. The proposed method was validated in terms of its limits of detection, limits of quantitation, linearity, precision, and accuracy. More specifically, the limits of detection of the four chromones ranged from 0.006 to 0.033 μg/mL, while the limits of quantitation ranged from 0.019 to 0.101 μg/mL. Our method also exhibited a good regression (r > 0.999), excellent precision (RSD < 0.60%), and acceptable recoveries (99.48-102.89%). Finally, the quantities of these four chromones present in 20 commercial samples from Korea and China were successfully evaluated using the developed method, indicating that the proposed method is suitable for the rapid and accurate quality control of Saposhnikovia divaricata.

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Peak deformations in preparative supercritical fluid chromatography due to co-solvent adsorption

Cited by 18 publications

References 49 publications

Opportunities and challenges of liquid chromatography coupled to supercritical fluid chromatography

Opportunities and challenges of liquid chromatography coupled to supercritical fluid chromatography

Impact of Methanol Adsorption on the Robustness of Analytical Supercritical Fluid Chromatography in Transfer from SFC to UHPSFC

Ultra‐performance convergence chromatography method for the determination of four chromones and quality control of Saposhnikovia divaricata (Turcz.) Schischk.

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