Skip to main content
SpringerLink
Log in

Quantification of free and esterified long-chain fatty acids without extraction by high-performance liquid chromatography in anaerobic digestion sludge

  • ORIGINAL ARTICLE
  • Published:
Journal of Material Cycles and Waste Management Aims and scope Submit manuscript

Abstract

During anaerobic digestion, the concentrations of long-chain fatty acids (LCFAs) need to be monitored to achieve good performance due to their adverse effects on the digestion process. LCFAs in anaerobic digester sludge are commonly analyzed by gas chromatography after extraction using an organic solvent. However, helium gas, which is used as the carrier gas during gas chromatography, has recently become difficult to obtain worldwide. Though helium-independent method for analyzing LCFAs in anaerobic digester sludge by high-performance liquid chromatography (HPLC) was described, the protocol was complex and not validated. Here, we developed new sample-preparation techniques, which was in conjunction with a modified version of an established HPLC technique. Notably, this method does not require an extraction process using a hazardous organic solvent. LCFAs in the sludge were dissolved in 2-propanol directly and then the sample was subjected to derivatization step. After validation, this method was applied to samples from anaerobic batch digestion of olive oil. Detailed analysis of LCFAs provided new insights into their hydrolysis kinetics according to acylglycerol content.

This is a preview of subscription content, log in via an institution to check access.

Access this article

Log in via an institution

Price excludes VAT (USA)
Tax calculation will be finalised during checkout.

Instant access to the full article PDF.

Institutional subscriptions

Fig. 1
Fig. 2
Fig. 3

Similar content being viewed by others

Data availability

The data that support the findings of this study are available from the corresponding author upon reasonable request.

References

  1. Xu F, Li Y, Ge X et al (2018) Anaerobic digestion of food waste—challenges and opportunities. Bioresour Technol 247:1047–1058. https://doi.org/10.1016/j.biortech.2017.09.020

    Article  Google Scholar 

  2. Salama ES, Saha S, Kurade MB et al (2019) Recent trends in anaerobic co-digestion: fat, oil, and grease (FOG) for enhanced biomethanation. Prog Energy Combust Sci 70:22–42. https://doi.org/10.1016/j.pecs.2018.08.002

    Article  Google Scholar 

  3. Hanaki K, Matsuo T, Nagase M (1981) Mechanism of inhibition caused by long-chain fatty acids in anaerobic digestion process. Biotechnol Bioeng 70:22–42. https://doi.org/10.1002/bit.260230717

    Article  Google Scholar 

  4. Weng C, Jeris JS (1976) Biochemical mechanisms in the methane fermentation of glutamic and oleic acids. Water Res. https://doi.org/10.1016/0043-1354(76)90151-2

    Article  Google Scholar 

  5. Lalman J, Bagley DM (2002) Effects of C18 long chain fatty acids on glucose, butyrate and hydrogen degradation. Water Res. https://doi.org/10.1016/S0043-1354(02)00014-3

    Article  Google Scholar 

  6. Stoll U, Gupta H (1997) Management strategies for oil and grease residues. Waste Manag Res. https://doi.org/10.1006/wmre.1996.0062

    Article  Google Scholar 

  7. Pereira MA, Pires OC, Mota M, Alves MM (2005) Anaerobic biodegradation of oleic and palmitic acids: evidence of mass transfer limitations caused by long chain fatty acid accumulation onto the anaerobic sludge. Biotechnol Bioeng 92:15–23. https://doi.org/10.1002/bit.20548

    Article  Google Scholar 

  8. Broughton MJ, Thiele JH, Birch EJ, Cohen A (1998) Anaerobic batch digestion of sheep tallow. Water Res 92:15–23. https://doi.org/10.1016/S0043-1354(97)00345-X

    Article  Google Scholar 

  9. Jarvis GN, Thiele JH (1997) High-performance liquid chromatographic analysis of free long chain fatty acids produced during lipolysis by anaerobic digestor sludge. J Chromatogr A. https://doi.org/10.1016/S0021-9673(96)00808-4

    Article  Google Scholar 

  10. Lalman JA, Bagley DM (2000) Anaerobic degradation and inhibitory effects of linoleic acid. Water Res. https://doi.org/10.1016/S0043-1354(00)00180-9

    Article  Google Scholar 

  11. Neves L, Pereira MA, Mota M, Alves MM (2009) Detection and quantification of long chain fatty acids in liquid and solid samples and its relevance to understand anaerobic digestion of lipids. Bioresour Technol. https://doi.org/10.1016/j.biortech.2008.06.018

    Article  Google Scholar 

  12. Procida G, Ceccon L (2006) Gas chromatographic determination of free fatty acids in olive mill waste waters. Anal Chim Acta. https://doi.org/10.1016/j.aca.2006.01.008

    Article  Google Scholar 

  13. Fernández A, Sánchez A, Font X (2005) Anaerobic co-digestion of a simulated organic fraction of municipal solid wastes and fats of animal and vegetable origin. Biochem Eng J. https://doi.org/10.1016/j.bej.2005.02.018

    Article  Google Scholar 

  14. Bligh EG, Dyer WJ (1959) A rapid method of total lipid extraction and purification. Can J Biochem Physiol. https://doi.org/10.1139/y59-099

    Article  Google Scholar 

  15. Cirne DG, Paloumet X, Björnsson L et al (2007) Anaerobic digestion of lipid-rich waste—effects of lipid concentration. Renew Energy 32:965–975. https://doi.org/10.1016/j.renene.2006.04.003

    Article  Google Scholar 

  16. Kaluzny MA, Duncan LA, Merritt MV, Epps DE (1985) Rapid separation of lipid classes in high yield and purity using bonded phase columns. J Lipid Res. https://doi.org/10.1016/s0022-2275(20)34412-6

    Article  Google Scholar 

  17. McCoy M (2022) Pfizer sues over trade secret theft. C&EN Glob Enterp 100:9–9. https://doi.org/10.1021/cen-10006-buscon3

    Article  Google Scholar 

  18. Miwa H, Yamamoto M (1996) Rapid liquid chromatographic determination of fatty acids as 2-nitrophenylhydrazine derivatives. J AOAC Int. https://doi.org/10.1093/jaoac/79.2.493

    Article  Google Scholar 

  19. Miwa H, Yamamoto M (1990) Liquid chromatographic determination of free and total fatty acids in milk and milk products as their 2-nitrophenylhydrazides. J Chromatogr A. https://doi.org/10.1016/0021-9673(90)85026-R

    Article  Google Scholar 

  20. Miwa H, Hiyama C, Yamamoto M (1985) high-performance liquid chromatography of short-and long-chain fatty acids as 2-nitrophenylhydrazides. J Chromatogr A. https://doi.org/10.1016/S0021-9673(01)90433-9

    Article  Google Scholar 

  21. Castillo MA, Castells RC (2001) Initial evaluation of quantitative performance of chromatographic methods using replicates at multiple concentrations. J Chromatogr A. https://doi.org/10.1016/S0021-9673(01)00867-6

    Article  Google Scholar 

  22. Shah VP, Midha KK, Dighe S et al (1992) Analytical methods validation: bioavailability, bioequivalence, and pharmacokinetic studies. J Pharm Sci. https://doi.org/10.1002/jps.2600810324

    Article  Google Scholar 

  23. Ziels RM, Karlsson A, Beck DAC et al (2016) Microbial community adaptation influences long-chain fatty acid conversion during anaerobic codigestion of fats, oils, and grease with municipal sludge. Water Res 103:372–382. https://doi.org/10.1016/j.watres.2016.07.043

    Article  Google Scholar 

  24. Gupta R, Gupta N, Rathi P (2004) Bacterial lipases: an overview of production, purification and biochemical properties. Appl Microbiol Biotechnol 64:763–781

    Article  Google Scholar 

  25. Ramos C, García A, Diez V (2014) Performance of an AnMBR pilot plant treating high-strength lipid wastewater: biological and filtration processes. Water Res. https://doi.org/10.1016/j.watres.2014.09.021

    Article  Google Scholar 

  26. Sakurai R, Takizawa S, Fukuda Y, Tada C (2021) Exploration of microbial communities contributing to effective methane production from scum under anaerobic digestion. PLoS ONE. https://doi.org/10.1371/journal.pone.0257651

    Article  Google Scholar 

Download references

Acknowledgements

This study was supported by BIOENERGY (Tokyo, Japan).

Author information

Authors and Affiliations

  1. Laboratory of Sustainable Animal Environment, Graduate School of Agricultural Science, Tohoku University, Osaki, Miyagi, Japan

    Riku Sakurai, Yoshimi Yokoyama, Yasuhiro Fukuda & Chika Tada

Authors
  1. Riku Sakurai
    View author publications

    You can also search for this author in PubMed Google Scholar

  2. Yoshimi Yokoyama
    View author publications

    You can also search for this author in PubMed Google Scholar

  3. Yasuhiro Fukuda
    View author publications

    You can also search for this author in PubMed Google Scholar

  4. Chika Tada
    View author publications

    You can also search for this author in PubMed Google Scholar

Corresponding author

Correspondence to Chika Tada.

Additional information

Publisher's Note

Springer Nature remains neutral with regard to jurisdictional claims in published maps and institutional affiliations.

Rights and permissions

Springer Nature or its licensor (e.g. a society or other partner) holds exclusive rights to this article under a publishing agreement with the author(s) or other rightsholder(s); author self-archiving of the accepted manuscript version of this article is solely governed by the terms of such publishing agreement and applicable law.

Reprints and permissions

About this article

Check for updates. Verify currency and authenticity via CrossMark

Cite this article

Sakurai, R., Yokoyama, Y., Fukuda, Y. et al. Quantification of free and esterified long-chain fatty acids without extraction by high-performance liquid chromatography in anaerobic digestion sludge. J Mater Cycles Waste Manag 25, 810–815 (2023). https://doi.org/10.1007/s10163-022-01561-z

Download citation

  • Received:

  • Accepted:

  • Published:

  • Issue Date:

  • DOI: https://doi.org/10.1007/s10163-022-01561-z

Keywords

Search

Navigation