Integrating a post-column makeup pump into preparative supercritical fluid chromatography systems to address stability and recovery issues during purifications

Bajpai, Lakshmikant; Naidu, Harshavardhan; Asokan, Kathiravan; Shaik, Khaja Mohiddin; Kaspady, Mahammed; Arunachalam, Piramanayagam; Wu, Dauh‐Rurng; Mathur, Arvind; Sarabu, Ramakanth

doi:10.1016/j.chroma.2017.06.063

Cited by 7 publications

(3 citation statements)

References 35 publications

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“…A make-up solvent can be introduced between the chromatograph and mass spectrometer to avoid solute precipitation inherent to CO 2 depressurization and generate a stable and homogeneous spray, thus improving ionization efficiency and detection sensitivity independently from chromatographic separation. , In this study, the chromatographic effluent was combined post-column with a make-up solvent containing a DIL reagent. The doubly charged DIL is expected to create ion pairing with the oppositely charged anionic PFC analytes via charge complexation during the ESI process.…”

Section: Resultsmentioning

confidence: 99%

Post-Chromatographic Dicationic Ionic Liquid-Based Charge Complexation for Highly Sensitive Analysis of Anionic Compounds by Ultra-High-Performance Supercritical Fluid Chromatography Coupled with Electrospray Ionization Mass Spectrometry

Chen

et al. 2020

Anal. Chem.

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A green analytical strategy has been developed for the analysis of 10 perfluorinated compounds (PFCs) incorporating supramolecular solvent (SUPRAS)-based extraction and ultra-high-performance supercritical fluid chromatography (UHPSFC)–tandem mass spectrometry. The SUPRAS was prepared through self-assembly of reverse micelles by mixing heptanol, tetrahydrofuran, and water at optimized volume ratios. An imidazolium-based germinal dicationic ionic liquid (DIL), 1,1-bis(3-methylimidazolium-1-yl) butylene difluoride ([C4(MIM)2]F2), was dissolved in the make-up solvent of UHPSFC and introduced post-column but before the electrospray ionization source. After chromatographic separation on a Torus DIOL analytical column (100 mm × 2.1 mm, 1.7 μm), the PFC analytes associated with the DIL reagent through charge complexation. The formation of positively charged complexes resulted in improved ionization efficiency and analytical sensitivity. Enhancement in signal intensity by one to two magnitudes was achieved in the positive ionization mode compared to the negative ionization mode without using the dicationic ion-pairing reagent. The developed protocol was applied to 32 samples of real textiles and 6 samples of real food packaging materials, which exhibited great potential for the analysis of anionic compounds.

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Section: Resultsmentioning

confidence: 99%

Post-Chromatographic Dicationic Ionic Liquid-Based Charge Complexation for Highly Sensitive Analysis of Anionic Compounds by Ultra-High-Performance Supercritical Fluid Chromatography Coupled with Electrospray Ionization Mass Spectrometry

Chen

et al. 2020

Anal. Chem.

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“…To provide an enantiomerically pure ibuprofen medication to maximize benefit and minimize risk to the patient, preparative purification methods are required. There are several methods to produce enantiomerically pure compounds including preparative highperformance liquid chromatography (HPLC), [11][12][13] supercritical fluid chromatography (SFC), [14][15][16] and diastereomeric crystallization. 17,18 Diastereomeric crystallization is a commonly applied technique, but it is often confined to a particular case, requiring reagents that are only effective for a particular system.…”

Section: Introductionmentioning

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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“…Now more than ever, analytical and preparative enantiomeric separations play a crucial role in industry and academic research [1]. There are a wide variety of methods to achieve and analyze enantiomerically pure compounds, including liquid chromatography (LC) [2,3], supercritical fluid chromatography [4,5,6], diastereomeric crystallization [7,8], membranes [9,10], asymmetric catalysis [11], simulated moving bed [12,13], dynamic and enzyme-mediated kinetic resolution [14,15], among others.…”

Section: Introductionmentioning

confidence: 99%

Chiral Stationary Phases for Liquid Chromatography: Recent Developments

et al. 2019

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The planning and development of new chiral stationary phases (CSPs) for liquid chromatography (LC) are considered as continuous and evolutionary issues since the introduction of the first CSP in 1938. The main objectives of the development strategies were to attempt the improvement of the chromatographic enantioresolution performance of the CSPs as well as enlarge their versatility and range of applications. Additionally, the transition to ultra-high-performance LC were underscored. The most recent strategies have comprised the introduction of new chiral selectors, the use of new materials as chromatographic supports or the reduction of its particle size, and the application of different synthetic approaches for preparation of CSPs. This review gathered the most recent developments associated to the different types of CSPs providing an overview of the relevant advances that are arising on LC.

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Integrating a post-column makeup pump into preparative supercritical fluid chromatography systems to address stability and recovery issues during purifications

Cited by 7 publications

References 35 publications

Post-Chromatographic Dicationic Ionic Liquid-Based Charge Complexation for Highly Sensitive Analysis of Anionic Compounds by Ultra-High-Performance Supercritical Fluid Chromatography Coupled with Electrospray Ionization Mass Spectrometry

Post-Chromatographic Dicationic Ionic Liquid-Based Charge Complexation for Highly Sensitive Analysis of Anionic Compounds by Ultra-High-Performance Supercritical Fluid Chromatography Coupled with Electrospray Ionization Mass Spectrometry

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

Chiral Stationary Phases for Liquid Chromatography: Recent Developments

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