Super/Subcritical Fluid Chromatography With Packed Columns: State of the Art and Applications

Silva, Carla Grazieli Azevedo da

doi:10.5935/0100-4042.20140158

Cited by 6 publications

(6 citation statements)

References 1 publication

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“…For instance, it has been reported that the formation of inclusion complexes between cyclodextrin CSPs and chiral analytes can be limited by the low polarity of the carbon dioxide mobile phase in pSFC [36]. On the other hand, chiral polysaccharide-based stationary phases have been widely used for pSFC enantioseparations due to the broad enantioselectivity that has been demonstrated for this CSP and separation technique [37]. Indeed, cellulose and amylose CSPs are reported to be effective CSPs in pSFC based on their chiral recognition ability [38] and were therefore selected for investigation in this study (CEL1, CEL2, and AMY1, specifically).…”

Section: Resultsmentioning

confidence: 99%

Enantioselective Analytical- and Preparative-Scale Separation of Hexabromocyclododecane Stereoisomers Using Packed Column Supercritical Fluid Chromatography

et al. 2016

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Hexabromocyclododecane (HBCDD) is an additive brominated flame retardant which has been listed in Annex A of the Stockholm Convention for elimination of production and use. It has been reported to persist in the environment and has the potential for enantiomer-specific degradation, accumulation, or both, making enantioselective analyses increasingly important. The six main stereoisomers of technical HBCDD (i.e., the (+) and (−) enantiomers of α-, β-, and γ-HBCDD) were separated and isolated for the first time using enantioselective packed column supercritical fluid chromatography (pSFC) separation methods on a preparative scale. Characterization was completed using published chiral liquid chromatography (LC) methods and elution profiles, as well as X-ray crystallography, and the isolated fractions were definitively identified. Additionally, the resolution of the enantiomers, along with two minor components of the technical product (δ-and ε-HBCDD), was investigated on an analytical scale using both LC and pSFC separation techniques, and changes in elution order were highlighted. Baseline separation of all HBCDD enantiomers was achieved by pSFC on an analytical scale using a cellulose-based column. The described method emphasizes the potential associated with pSFC as a green method of isolating and analyzing environmental contaminants of concern.

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Section: Resultsmentioning

confidence: 99%

Enantioselective Analytical- and Preparative-Scale Separation of Hexabromocyclododecane Stereoisomers Using Packed Column Supercritical Fluid Chromatography

et al. 2016

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“…Despite the advantages of SFC over HPLC and GC, SFC has one of the biggest limitations. It is not able to analyze extremely polar samples due to the nonpolar mobile phase ( Silva and Collins, 2014 ). CO 2 lacks of polarity and hence it may be quite challenging to elute polar compounds from the stationary phase ( Pavan and Raja, 2020 ).…”

Section: Stability Indicating Assaysmentioning

confidence: 99%

Choices of chromatographic methods as stability indicating assays for pharmaceutical products: A review

Chew

Khor

Lim

2021

Heliyon

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Stability indicating assay describes a technique which is used to analyse the stability of drug substance or active pharmaceutical ingredient (API) in bulk drug and pharmaceutical products. Stability indicating assay must be properly validated as per ICH guidelines. The important components in a stability indicating assay include sensitivity, specificity, accuracy, reliability, reproducibility and robustness. A validated assay is able to measure the concentration changes of drug substance/API with time and make reliable estimation of the quantity of the degradation impurities. The drug substance is separated and resolved from the impurities. Pros and cons of HPLC, GC, HPTLC, CE and SFC were discussed and reviewed. Stability indicating assay may consist of the combination of chromatographic separation and spectroscopic detection techniques. Hyphenated system could demonstrate parallel quantitative and qualitative analysis of drug substances and impurities. Examples are HPLC-DAD, HPLC-FL, GC-MS, LC-MS and LC-NMR. The analytes in the samples are separated in the chromatography while the impurities are chemically characterised by the spectroscopy in the system. In this review, various chromatographic methods which had been employed as stability indicating assays for drug substance and pharmaceutical formulation were systematically reviewed, and the application of hyphenated techniques in impurities characterisation and identification were also discussed with supporting literatures.

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“…Ammonia was added because basic additives are commonly used to improve peak shape and efficiency in SFC chiral separations. 28,29 The modifier gradient conditions were 7% (at t=0), 7-55% (from t=1 to t=8) and 7% (at t=8.01). As shown in Figure 1, Chiralcel OX-H® demonstrated the best separation among the seven CSPs.…”

Section: Analytical Sfcmentioning

confidence: 99%

Rapid Purification of Drug Enantiomers using Supercritical Fluid Chromatographic Method: Ibuprofen as a Model Compound

Lee¹,

Gahm²,

Jin³

et al. 2021

IJPER

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Background:The purification of drug enantiomers is an essential technique because pharmacological activity differs depending on individual enantiomers. Nowadays, supercritical fluid technology is utilized for various purposes in the pharmaceutical field. Methodology: In this study, an efficient and streamlined method development strategy for finding an effective analytical method in supercritical fluid chromatography (SFC) is presented in detail for scaling up to preparative scale and achieving enantiomerically pure product, using ibuprofen as a model compound. Results: Through the optimized preparative method presented, the individual (R) enantiomer of the commercial racemate of ibuprofen can be obtained with a recovery yield of 80.0% and an enantiomeric excess of 95.1 and the individual (S) enantiomer can be obtained with a recovery yield of 77.6% with an enantiomeric excess of 99.3, respectively. Conclusion: The use of analytical and preparative SFC systems has advantages over the conventional chromatography systems in terms of separation time, reduced solvent consumption and high productivity for ibuprofen's enantiomeric purification.

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Super/Subcritical Fluid Chromatography With Packed Columns: State of the Art and Applications

Cited by 6 publications

References 1 publication

Enantioselective Analytical- and Preparative-Scale Separation of Hexabromocyclododecane Stereoisomers Using Packed Column Supercritical Fluid Chromatography

Enantioselective Analytical- and Preparative-Scale Separation of Hexabromocyclododecane Stereoisomers Using Packed Column Supercritical Fluid Chromatography

Choices of chromatographic methods as stability indicating assays for pharmaceutical products: A review

Rapid Purification of Drug Enantiomers using Supercritical Fluid Chromatographic Method: Ibuprofen as a Model Compound

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