Solid phase extraction on reverse phase chromatographic media subjected to stresses expected for extraterrestrial implementation

Ferrance, Jerome P.

doi:10.1039/d2an00768a

Cited by 2 publications

(6 citation statements)

References 29 publications

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“…The Oasis MCX strong cation exchange media selected is built on the Oasis HLB hydrophilic−lipophilic particles that were utilized in reversedphase extractions of these same analytes. 22 Thermal/vacuum and sonication testing of the HLB particles showed no loss of functionality, and they were not affected by radiation or longterm cold storage, suggesting that these phases should be stable to spaceflight conditions. Initial experiments with the Oasis MCX media-packed columns showed both fluorescent and absorption signals (in addition to the normal background absorption/fluorescence from the ocean water simulant blank) in most fractions from blank extractions loading only IO solution.…”

Section: Cation Exchange Testing 311 Single Analytementioning

confidence: 90%

“…The Oasis HLB backbone of the MCX particles had been thermal and vacuum tested in the previous work, but it was important to perform the radiation/frozen storage tests that highlighted issues with some of the reversed-phase media observed in that work. 22 Fifteen columns were packed with the Oasis MCX media using three different media lots, with the amounts packed ranging from 220 to 270 mg. All columns were tested before irradiation for extraction of leucine and γ-aminobutyric acid (GABA) from IO solution. Once irradiated, the columns were again tested using these same two analytes to show that capture and elution of the analytes had not been affected by the irradiation procedure.…”

Section: Radiation and Storagementioning

confidence: 99%

“…The present work has taken a different approach. The ion exchange phases selected were specifically designed for SPE and are built on the hydrophilic/lipophilic backbone of the Oasis hydrophobic-lipophilic balance (HLB) particles used in our earlier reversed-phase work . This provides these phases with true mixed-mode capture characteristics of both reversed-phase and ion exchange.…”

Section: Introductionmentioning

confidence: 99%

“…The ion exchange phases selected were specifically designed for SPE and are built on the hydrophilic/lipophilic backbone of the Oasis hydrophobic-lipophilic balance (HLB) particles used in our earlier reversed-phase work. 22 This provides these phases with true mixed-mode capture characteristics of both reversed-phase and ion exchange. In addition to simply focusing on amino acids for this work, organic acids and amines, nucleobases, peptides, and oligonucleotides, other potential organic biosignatures, were also evaluated for extraction and desalting using this method.…”

Section: Introductionmentioning

confidence: 99%

“…Our earlier work explored reversed-phase matrices for solid-phase extraction of potential analytes of interest, but these phases captured only a few of the small, polar analytes that are of interest as potential biomarker signatures . SPE using ion exchange media to capture small charged amino acids from inorganic salt solutions has been evaluated for a number of years using both cation and anion exchange resins. − Dreze et al proposed desalting of retained cationic analytes by first releasing the captured salt cations before eluting the analytes of interest.…”

Section: Introductionmentioning

confidence: 99%

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Testing of Ion Exchange Solid Phase Extraction Media for Extraterrestrial In Situ Sample Preparation on Liquid Samples

Ferrance

2023

ACS Earth Space Chem.

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The search for life on other bodies in our solar system is currently focused on Ocean Worlds, those bodies known to contain liquid water, as water is one of the requirements for life as we understand it. In the search for organic biosignatures that would indicate the presence of past or current life, liquid samples from these bodies would utilize an initial sample preparation step in which interfering substances such as salts can be removed before analysis. Previous work on potential sample preparation techniques for these samples evaluated solid phase extraction (SPE) on cation exchange media, but only explored amino acid analytes at low salt to analyte ratios and used high concentration eluents. This work utilized mixed-mode ion exchange solid phases, developing methods for elutions in low concentration solutions and evaluating polar analytes with a range of functionalities. Method development revealed the need for a pre-elution step in the process to decrease the elution volume required. Both anion and cation exchange media were evaluated for the capture of analytes from solutions that simulated Earth’s oceans. The Oasis MCX and Strata X-C cation exchange media provided the best results, with >90% retention of all analytes including amino acids, organic amines, nucleotides, peptides, and an oligonucleotide. These cation exchange media retained even anionic components, including glutamic acid and organic acids, with >90% efficiency. These analytes were released in the wash step, but salt ion removal was completed before release, allowing this technique to be used for desalting of these analytes. Extraction of a 14 component mixed analyte solution also showed retention of all analytes, with testing of analyte concentrations down to 100 nM in 35 g/L simulated ocean solution. Oasis MAX and Strata X-A anion exchange media did not retain glutamic acid, fumaric acid, or dipicolinic acid when the salt concentration was high; these anionic analytes were easily extracted from low salt solutions. The anion exchange media showed a range of functionality for extracting other analytes from the simulated ocean water, capturing >90% of tryptophan and phenylalanine, but retaining <50% of the valine and >20% of the glycine. Irradiation exposure, as a model for the solar irradiation expected during deployment to extraterrestrial locations, did not affect the performance of any ion exchange media tested. A reversed-phase SPE column was directly coupled to a cation exchange column, to investigate removal of nonpolar compounds that might bind to and block the mixed-mode ion exchange media.

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Section: Cation Exchange Testing 311 Single Analytementioning

confidence: 90%

Section: Radiation and Storagementioning

confidence: 99%

Section: Introductionmentioning

confidence: 99%

Section: Introductionmentioning

confidence: 99%