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Figure 4. Our new extraction instrument has been installed and tested in an online

configuration with diode array and mass spectrometer detectors. We are currently

optimizing the pre-concentrator and extract transfer portion of the instrument. We

plan to add the chromatography column for SFC analysis in 2018.

Current on-line detectors installed in our system include a commercial diode array detector (190-900 nm, deuterium and tungsten) and mass spectrometer (ESI and APCI Sources, 10-2000 m/z). These detectors can be swapped for future state-of-the-art mass spectrometers or other instrumentation. A matured and miniaturized flight version of this instrument with ten sample cells would measure approximately 24”x28”x24”, weigh ~38 kg, and draw a maximum of 70 W of power (set by the mass spectrometer). While our COLDTech effort focuses instead on demonstrating potential science return for aqueous analysis and chromatography, the overall mass, size, and power requirements for miniaturization of this instrument in the future should be comparable.

Planetary science life-detection instrumentation has thus far depended on high-temperature extraction and detection methods that degrade organics and complicate the analysis. In some cases, these issues have led to confusing or ambiguous results. For example, the elevated temperatures required by pyrolysis techniques have been shown to cause reactions of organics with perchlorate salts in the Mars regolith to produce chlorohydrocarbons (detected by in situ instruments on Mars). Over the past decade, our team has worked to develop a low temperature method for extraction of polar and nonpolar organics that uses supercritical carbon dioxide as a ‘green’ solvent [McCaig et al. 2016, Menlyadiev et al. 2017). It was originally designed with Mars applications in mind, and we have successfully used it to extract fatty acids and amino acids from Mars regolith analogs without degradation of organics. Extraction with supercritical CO2 could sidestep some of the major analytic challenges from conventional techniques such as pyrolysis and conventional liquid extractions. The goals of this project are the following: Year 1: Integrate supercritical CO2 chromatography column and detector back-end (commercially available) with our front-end extractor, and demonstrate on-line detection following extraction with water+SCCO2. (completed) Year 2: Demonstrate extraction (and chiral separation) of chiral species from salty/icy/rocky materials to expand the range of acceptable sample types.

© 2017 California Institute of Technology.

Government sponsorship acknowledged.

Bryana L. Henderson, Fang Zhong, Victor Abrahamsson, Isik Kanik, Ying Lin, Jet Propulsion Laboratory, California Institute of Technology, Pasadena, CA

Life Detection for Ocean Worlds through Supercritical CO2 Extraction and Chiral Supercritical Fluid Chromatography

BACKGROUND ABSTRACT With future in situ missions to Ocean

Worlds now within reach, robust

instrumentation technologies are needed

for extraction and analysis of biomarkers

and chiral species (one of the key indicators

of extant life) from complex or unknown

matrix materials.

Supercritical CO2, a stable inorganic fluid

with ideal extraction properties, can be

easily combined with chromatography to

extract and separate a wide variety of

organics, including chiral species, from

complex sample materials without

derivatization.

We are currently developing a Supercritical

CO2 Extraction Supercritical Fluid

Chromatography (SCE-SFC) online benchtop

instrument in a proof-of-concept study

(entry TRL = 2; exit TRL = 4) for extraction

of relevant chiral biomarkers from aqueous

or mixed samples with minimal sample

preparation and minimal organic solvent

waste.

Lemmon, E., M. McLinden and M. Huber (2002). "Fluid thermodynamic and

transport properties." NIST Standard Reference Database 23, Version 7.0,

National Institute of Standards and Technology.

McCaig, H. C., A. Stockton, C. Crilly, S. Chung, I. Kanik, Y. Lin and F. Zhong

(2016). "Supercritical Carbon Dioxide Extraction of Coronene in the Presence

of Perchlorate for In Situ Chemical Analysis of Martian Regolith." Astrobiology.

Menlyadiev, M., B. L. Henderson, F. Zhong, Y. Lin and I. Kanik (2017). "Extraction

of Amino Acids using Supercritical Carbon Dioxide for in Situ Chemical

Analysis for Astrobiological Applications." Accepted, International Journal of

Astrobiology.

White, C. (2005). "Integration of supercritical fluid chromatography into drug

discovery as a routine support tool: Part I. Fast chiral screening and

purification." Journal of Chromatography A 1074(1): 163-173.

Figure 1. Our SCE-SFC instrument will extract organics from complex matrix materials regardless of their composition

(mixed ice + regolith, salty aqueous ocean mixtures, sludge, sand, rock, etc.) This expanded field of allowable sample

types reduces risk in cases where the surface composition is unknown.

REFERENCES

ACKNOWLEDGMENTS

CONTACT Bryana L. Henderson Jet Propulsion Lab,

California Institute of Technology Email: Bryana.L.Henderson@jpl.nasa.gov

This research was enabled through funding from

NASA’s Concepts for Ocean Worlds Life Detection

Technology (COLDTech) Program and prior funding

from NASA’s Astrobiology Science and Technology

Instrument Development (ASTID) Program. This

research was carried out at the Jet Propulsion

Laboratory, California Institute of Technology,

under a contract with the National Aeronautics

and Space Administration.

Photo credit | Galileo Project, JPL, NASA, Ted Stryk Photo credit | ESA

MARS

ICE, ROCK, REGOLITH, EVAPORITES…

EUROPA

ICE, SALT, REGOLITH?

SFC is taking over as the industry standard in the pharmeceutical, food, and petroleum industries. SFC is considered to be the best chiral separation technique available.

Other advantages of this SFC technique:

(1) It can be used to analyze both nonpolar and polar species,

(2) Many types of columns are available for purchase commercially,

(3) It allows for analysis of nonvolatiles without sample derivitization (as in GC-MS), and

(4) It has the same benefits of HPLC but does not require large volumes of solvent and mass and power because each sample takes significantly less time to analyze and has higher efficiency (see Figure 3). It has been used to increase analysis speed by up to 15x [White 2005].

SCE uses pressurized warm carbon dioxide (>1070 psi and >31 C; see Figure 2) as a solvent to extract from a matrix. SFE has the following advantages:

(1) No harsh organic solvents are needed (no special hydrocarbon or chlorinated waste considerations)

(2) CO2 gas is inert and can be vented directly to air,

(3) No sample preparation is needed, and

(4) No high temperatures are needed.

ADVANTAGES OF SUPERCRITICAL CO2 EXTRACTION (SCE)

Figure 2. CO2 phase

diagram [NIST Standard

Reference Database 23,

Version 9.1]. Compared to

regular organic solvents,

supercritical CO2 has one

order of magnitude higher

diffusivity, one order of

magnitude lower viscosity,

and near zero surface

tension.

Combined with the extraction advantages of supercritical CO2, the SCE-SFC combination proposed

here is ideal for in situ detection of organics and biomarkers on Ocean Worlds.

Figure 3. Chiral separation of trans-stilbene oxide using HPLC (top) and

SFC (bottom), both using the same chiral column for separation (Image

from JASCO). Because of the superior transfer properties of supercritical

CO2, supercritical fluid chromatography can separate chiral enantiomers in

much less time and with better resolution than HPLC.

SCE-SFE INTEGRATED INSTRUMENT ADVANTAGES OF SUPERCRITICAL FLUID CHROMATOGRAPHY (SFC)