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High-Throughput Analysis of Algal Crude Oils Using High Resolution Mass Spectrometry

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Lipids

Abstract

Lipid analysis often needs to be specifically optimized for each class of compounds due to its wide variety of chemical and physical properties. It becomes a serious bottleneck in the development of algae-based next generation biofuels when high-throughput analysis becomes essential for the optimization of various process conditions. We propose a high-resolution mass spectrometry-based high-throughput assay as a ‘quick-and-dirty’ protocol to monitor various lipid classes in algal crude oils. Atmospheric pressure chemical ionization was determined to be most effective for this purpose to cover a wide range of lipid classes. With an autosampler-LC pump set-up, we could analyze algal crude samples every one and half minutes, monitoring several lipid species such as TAG, DAG, squalene, sterols, and chlorophyll a. High-mass resolution and high-mass accuracy of the orbitrap mass analyzer provides confidence in the identification of these lipid compounds. MS/MS and MS3 analysis could be performed in parallel for further structural information, as demonstrated for TAG and DAG. This high-throughput method was successfully demonstrated for semi-quantitative analysis of algal oils after treatment with various nanoparticles.

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Abbreviations

APCI:

Atmospheric pressure chemical ionization

AP-MSN-3:

Aminopropyl functionalized mesoporous silica nanoparticles with 3 nm pore size

AP-MSN-5:

Aminopropyl functionalized mesoporous silica nanoparticles with 5 nm pore size

AP-MSN-10:

Aminopropyl functionalized mesoporous silica nanoparticles with 10 nm pore size

APPI:

Atmospheric pressure photoionization

CHCA:

α-Cyano-4-hydroxycinnamic acid

CID:

Collision-induced dissociation

CTAB:

Cetyl trimethylammonium bromide

DAG:

Diacylglycerols

ESI:

Electrospray ionization

FFA:

Free fatty acids

FTICRMS:

Fourier transform ion cyclotron resonance mass spectrometer

GC:

Gas chromatography

HPLC:

High performance liquid chromatography

HRMS:

High resolution mass spectrometry

MALDI:

Matrix-assisted laser desorption ionization

MS:

Mass spectrometry

MS/MS:

Tandem mass spectrometry

MS3:

MS/MS/MS, triple stage tandem mass spectrometry

MSN-10:

Mesoporous silica nanoparticles with 10 nm pore size

SPE:

Solid phase extraction

TAG:

Triacylglycerols

TEOS:

Tetraethylorthosilicate

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Acknowledgments

We thank Adam Klein for his help in setting up the autosampler-LC configuration. This work is supported by U.S. Department of Energy, Office of Energy Efficiency and Renewable Energy (DE-FG26-0NT08854). The Ames Laboratory is operated by Iowa State University under DOE Contract DE-AC02-07CH11358.

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Author notes

  1. Brian G. Trewyn

    Present address: Department of Chemistry and Geochemistry, Colorado School of Mines, Golden, CO, 80401, USA

Authors and Affiliations

  1. U.S.-DOE Ames Laboratory, Ames, IA, 50011, USA

    Young ** Lee, Rachael C. Leverence, Erica A. Smith, Justin S. Valenstein, Kapil Kandel & Brian G. Trewyn

  2. Department of Chemistry, Iowa State University, Ames, IA, 50011, USA

    Young ** Lee, Erica A. Smith, Justin S. Valenstein, Kapil Kandel & Brian G. Trewyn

Authors
  1. Young ** Lee
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  2. Rachael C. Leverence
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  4. Justin S. Valenstein
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Corresponding author

Correspondence to Young ** Lee.

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Lee, Y.J., Leverence, R.C., Smith, E.A. et al. High-Throughput Analysis of Algal Crude Oils Using High Resolution Mass Spectrometry. Lipids 48, 297–305 (2013). https://doi.org/10.1007/s11745-013-3757-7

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  • DOI: https://doi.org/10.1007/s11745-013-3757-7

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