Evaluation of temperature and pressure effects on retention in supercritical fluid chromatography on polar stationary phases

Ovchinnikov, D. V.; Pokrovskiy, O. I.; Kosyakov, D. S.; Боголицын, К. Г.; Ul’yanovskii, N. V.; Falev, Danil I.

doi:10.1016/j.chroma.2019.460600

Cited by 17 publications

(7 citation statements)

References 31 publications

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“…Variations of temperature (20–55 °C) and backpressure (110–190 bar) did not significantly affect the separation of triterpenoids on an HSS C18 SB column, which is in good agreement with the published data on the minority of these parameters when optimizing separation in SFC on polar stationary phases [ 31 ]. To ensure the maximum chromatographic column lifetime and the stability of maintaining the temperature, we chose 25 °C as the optimal value.…”

Section: Resultssupporting

confidence: 88%

“…Due to the low viscosity and thus high diffusion coefficients of such media, SFC features high mass transfer rate, higher efficiency, and exceptional separation speed. It has been successfully used for rapid analysis of various natural compounds [ 29 , 30 , 31 , 32 ]. There are few published works on the use of SFC for the analysis of PCTs; the most recent one [ 33 ] uses a combination of SFC with light scattering detection (ELSD).…”

Section: Introductionmentioning

confidence: 99%

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Supercritical Fluid Chromatography—Tandem Mass Spectrometry for Rapid Quantification of Pentacyclic Triterpenoids in Plant Extracts

et al. 2022

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Pentacyclic triterpenoids (PCTs) are a widely distributed class of plant secondary metabolites. These compounds have high bioactive properties, primarily antitumor and antioxidant activity. In this study, a method was developed for the quantitative analysis of pentacyclic triterpenoids in plants using supercritical fluid chromatography–tandem mass spectrometry (SFC-MS/MS). Separation of ten major PCTs (friedelin, lupeol, β-amyrin, α-amyrin, betulin, erythrodiol, uvaol, betulinic, oleanolic and ursolic acids) was studied on six silica-based reversed stationary phases. The best results (7 min analysis time in isocratic elution mode) were achieved on an HSS C18 SB stationary phase using carbon dioxide—isopropanol (8%) mobile phase providing decisive contribution of polar interactions to the retention of analytes. It was shown that the use of atmospheric pressure chemical ionization (APCI) is preferred over atmospheric pressure photoionization (APPI). The combination of SFC with APCI-MS/MS mass spectrometry made it possible to achieve the limits of quantification in plant extracts in the range of 2.3–20 μg·L−1. The developed method was validated and tested in the analyses of birch outer layer (Betula pendula) bark, and licorice (Glycyrrhiza glabra) root, as well as lingonberry (Vaccinium vitis-idaea), cranberry (Vaccinium oxycoccos), apple (Malus domestica “Golden Delicious” and Malus domestica “Red Delicious”) peels.

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Section: Resultssupporting

confidence: 88%

Section: Introductionmentioning

confidence: 99%

Supercritical Fluid Chromatography—Tandem Mass Spectrometry for Rapid Quantification of Pentacyclic Triterpenoids in Plant Extracts

et al. 2022

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“…Temperature and backpressure usually do not have a significant effect on SFC separations with polar stationary phases and are often considered as secondary parameters when optimizing a chromatographic method [ 33 ]. Indeed, we noted some improvement in the chromatographic peak shapes (especially for FADMH) and a slight decrease in retention times with an increase in backpressure, which can be partially compensated by an increase in temperature.…”

Section: Resultsmentioning

confidence: 99%

“…PLE of all soil samples with acetonitrile was carried out using an ASE-350 (Dionex, Sunnyvale, CA, USA) accelerated solvent extraction system in nitrogen atmosphere according to the earlier developed procedure [ 33 ] briefly described below.…”

Section: Methodsmentioning

confidence: 99%

Rapid Simultaneous Quantification of 1-Formyl-2,2-Dimethylhydrazine and Dimethylurea Isomers in Environmental Samples by Supercritical Fluid Chromatography–Tandem Mass Spectrometry

et al. 2022

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When released to the environment, the rocket fuel unsymmetrical dimethylhydrazine (UDMH) undergoes oxidative transformations, resulting in the formation of an extremely large number of nitrogen-containing transformation products, including isomeric compounds which are difficult to discriminate by common chromatography techniques. In the present work, supercritical fluid chromatography–tandem mass spectrometry (SFC-MS/MS) was proposed for resolving the problem of fast separation and simultaneous quantification of 1-formyl-2,2-dimethylhydrazine (FADMH) as one of the major UDMH transformation products, and its isomers—1,1-dimethylurea (UDMU) and 1,2-dimethylurea (SDMU). 2-Ethylpyridine stationary phase provided baseline separation of analytes in 1.5 min without the distortion of the chromatographic peaks. Optimization of SFC separation and MS/MS detection conditions allowed for the development of rapid, sensitive, and “green” method for the simultaneous determination of FADMH, UDMU, and SDMU in environmental samples with LOQs of 1–10 µg L−1 and linear range covering three orders of magnitude. The method was validated and successfully tested on the real extracts of peaty and sandy soils polluted with rocket fuel and UDMH oxidation products. It was shown that both UDMU and SDMU are formed in noticeable amounts during UDMH oxidation. Despite relatively low toxicity, UDMU can be considered one of the major UDMH transformation products and a potential marker of soil pollution with toxic rocket fuel.

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“…Ovchinnikov et al evaluated effects of temperatures (25‐55°C) and pressures (11‐18 MPa) on the analyte retention and the selectivity of 89 compounds from various chemical classes using four polar stationary phases (e.g. ethylene‐bridged hybrid silica, cyanopropyl, 2‐ethylpyridine, and zwitterionic sulfobetaine) 83 . It was found that only a moderate effect on the selectivity was observed, and increasing the pressure at constant temperatures increased the mobile phase density and its eluting power, hence decreasing the retention of all compounds.…”

Section: Packed Column Supercritical Fluid Chromatographymentioning

confidence: 99%

A review of retention mechanism studies for packed column supercritical fluid chromatography

Si-Hung

Bamba

2021

Analytical Science Advances

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The packed column supercritical fluid chromatography has risen as a promising alternative separation technique to the conventional liquid chromatography and gas chromatography. Although the packed column supercritical fluid chromatography has many advantages compared to other chromatographic techniques, its separation mechanism is not fully understood due to the complex combination effects of many chromatographic parameters on separation quality and the lacking of global strategies for studying separation mechanisms. This review aims to provide recent information regarding the chromatographic behaviors and the effects of the parameters on the separation, discuss the results, and point out the remaining bottlenecks in the packed column supercritical fluid chromatography retention mechanism studies.

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Evaluation of temperature and pressure effects on retention in supercritical fluid chromatography on polar stationary phases

Cited by 17 publications

References 31 publications

Supercritical Fluid Chromatography—Tandem Mass Spectrometry for Rapid Quantification of Pentacyclic Triterpenoids in Plant Extracts

Supercritical Fluid Chromatography—Tandem Mass Spectrometry for Rapid Quantification of Pentacyclic Triterpenoids in Plant Extracts

Rapid Simultaneous Quantification of 1-Formyl-2,2-Dimethylhydrazine and Dimethylurea Isomers in Environmental Samples by Supercritical Fluid Chromatography–Tandem Mass Spectrometry

A review of retention mechanism studies for packed column supercritical fluid chromatography

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