Skip to main content

Advertisement

Log in

Microwave-Assisted Methodology Feasibility for One-Step Extraction and Transmethylation of Fatty Acids in Milk for GC-Mass Spectrometry

  • Published:
Food Analytical Methods Aims and scope Submit manuscript

Abstract

Fatty acids (FAs) play many essential roles in biological systems, and they are the aim of different research studies due to their benefits on human health. Milk and dairy products contribute significantly to the consumption of FAs in the human diet. In consequence, manipulation of FA composition of cows’ milk via nutritional strategies has been an important target for the dairy industry and a challenge from an analytical point of view. Milk FA composition is complex, and their analysis involves multiple steps (extraction procedure, methylation, FA methyl ester extraction and gas chromatography (GC) determination) that turn it into a tedious and time-consuming procedure. In recent years, some efforts have been made to develop an analytical approach with simultaneous extraction and derivatization of FAs. In this sense, microwave (MW)-assisted digestion and extraction methods have been used for many years and today can be considered standard operating procedures in many laboratories. It is a powerful tool for different analytical methodology development. This study is focused on one-step extraction/transmethylation MW-assisted methodology feasibility for FA analysis in milk compared to a reference method.

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

Access this article

Subscribe and save

Springer+
from $39.99 /Month
  • Starting from 10 chapters or articles per month
  • Access and download chapters and articles from more than 300k books and 2,500 journals
  • Cancel anytime
View plans

Buy Now

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

Instant access to the full article PDF.

Similar content being viewed by others

References

  • Araujo P, Nguyen T, Froyland L, Wang J, Kang J (2008) Evaluation of a rapid method for the quantitative analysis of fatty acids in various matrices. J Chromatogr A 1212:106–113

    Article  CAS  Google Scholar 

  • Chen S, Bobe G, Zimmerman S, Hammond EG, Luhman CM, Boylston TD, Freeman AE, Beitz DC (2004) Physical and sensory properties of dairy products from cows with various milk fatty acid compositions. J Agric Food Chem 52:3422–3428

    Article  CAS  Google Scholar 

  • Chen J, Cao Y, Gao H, Yang L, Chen Z (2007) Isomerization of conjugated linolenic acids during methylation. Chem Phys Lipids 150:136–142

    Article  CAS  Google Scholar 

  • Chilliard Y, Ferlay A (2004) Dietary lipids and forages interactions on cow and goat milk fatty acid composition and sensory properties. Reprod Nutr Dev 44:467–492

    Article  CAS  Google Scholar 

  • Chouinard PY, Corneau L, SAEBØ A, Bauman DE (1999) Milk yield and composition during abomasal infusion of conjugated linoleic acids in dairy cows. J Dairy Sci 82:2737–2745

    Article  CAS  Google Scholar 

  • Christie WW (1982) A simple procedure for rapid transmethylation of glycerolipids and cholesteryl esters. J Lipid Res 23:1072–1075

    CAS  Google Scholar 

  • Collomb M, Schmid A, Sieber R, Wechsler D, Ryhanen EL (2006) Conjugated linoleic acids in milk fat: variation and physiological effects. Int Dairy J 16:1347–1361

    Article  CAS  Google Scholar 

  • Delmonte P, Fardin-Kia AR, Kramer JKG, Mossoba MM, Sidisky L, Tyburczy C, Arder JI (2012) Evaluation of highly polar ionic liquid gas chromatographic column for the determination of the fatty acids in milk fat. J Chromatogr A 1233:137–146

    Article  CAS  Google Scholar 

  • Demment MW and Allen LH (2004) Animal source foods to improve micronutrient nutrition and human function in developing countries. J Nutr 133 (Suppl.) 11-S II

  • Elgersma A, Tamminga S, Ellen G (2006) Modifying milk composition through forage. Anim Feed Sci Technol 131:207–225

    Article  CAS  Google Scholar 

  • Eskilsson CS, Bjorklund E (2000) Analytical-scale microwave-assisted extraction. J Chromatogr A 902:227–250

    Article  CAS  Google Scholar 

  • Feng S, Lock AL, Garnsworthy PC (2004) Technical note: a rapid lipid separation method for determining fatty acid composition of milk. J Dairy Sci 87(11):3785–3788

    Article  CAS  Google Scholar 

  • Glasser F, Ferlay A, Chilliard Y (2008) Oilseed lipid supplements and fatty acid composition of cow milk: a meta-analysis. J Dairy Sci 91(12):4687–4703

    Article  CAS  Google Scholar 

  • Giua L, Blasi F, Simonetti MS, Cossignani L (2013) Oxidative modifications of conjugated and unconjugated linoleic acid during heating. Food Chem 140:680–685

    Article  CAS  Google Scholar 

  • Hernández-Ortega M, Martínez-Fernández A, Soldado A, González A, Arriaga-Jordán CM, Argamentería A, de la Roza-Delgado B and Fernando V (2014) Effect of total mixed ration composition and daily grazing pattern on milk production, composition and fatty acids profile of dairy cows. J Dairy Res (available on CJO2014. doi:10.1017/S0022029914000399

  • Herzallah SM, Humeid MA, Al-Ismail KM (2005) Effect of heating and processing methods of milk and dairy products on conjugated linoleic acid and trans fatty acid isomer content. J Dairy Sci 88:1301–1310

    Article  CAS  Google Scholar 

  • International Standard ISO15884/IDF182. Milk fat-preparation of fatty acid methyl esters

  • International Standard ISO15885/IDF184. Milk fat-determination of the fatty acid composition by gas-liquid chromatography

  • Kalinin A, Krasheninnikov V (2014) Can a hand-held near infrared spectrometer serve as an analyser of dietary fatty acids? NIR News 25:16–18

    Article  Google Scholar 

  • Khoomrung S, Chumnanpuen P, Jansa-ard S, Nookaew I, Nielsen J (2012) Fast and accurate preparation fatty acid methyl esters by microwave-assisted derivatization in the yeast Saccharomyces cerevisiae. Appl Microbiol Biotechnol 94:1637–1646

    Article  CAS  Google Scholar 

  • Kramer JKG, Cruz-Hernandez C, Deng Z, Zhou J, Jahreis G, Dugan MER (2004) Analysis of conjugated linoleic acid and trans 18:1 isomers in synthetic and animal products1,2,3,4. Am J Clin Nutr 79:1137S–1145S

    CAS  Google Scholar 

  • Kramer JKG, Fellner V, Dugan MER, Sauer FD, Mossoba MM, Yurawecz MP (1997) Evaluating acid and base catalyst in the methylation of milk and rumen fatty acids with special emphasis on conjugated dienes and total trans fatty acids. Lipids 32:1219–1228

    Article  CAS  Google Scholar 

  • Kramer JKG, Hernández M, Cruz-Hernández C, Kraft J, Dugan MER (2008) Combining results of two GC separations partly achieves determination of all cis and trans 16:1, 18:1, 18:2 and 18:3 except CLA isomers of milk fat as demonstrated using Ag-Ion SPE fractionation. lipids 43:259–273

    Article  CAS  Google Scholar 

  • Liu R, Zhang J, Mou Z, Haob S, Zhang Z (2012) Microwave-assisted one-step extraction-derivatization for rapid analysis of fatty acids profile in herbal medicine by gas chromatography-mass spectrometry. Analyst 137:5135–5143

    Article  CAS  Google Scholar 

  • Luna P, Juarez M, de la Fuente MA (2008) Gas chromatography and silver-ion high-performance liquid chromatography analysis of conjugated linoleic acid isomers in free fatty acid form using sulphuric acid in methanol as catalyst. J Chromatogr A 1204:110–113

    Article  CAS  Google Scholar 

  • Moltó-Puigmartí C, Castellote AI, López-Sabater MC (2007) Conjugated linoleic acid determination in human milk by fast – gas chromatography. Anal Chim Acta 602:122–130

    Article  Google Scholar 

  • Morales-Almaraz E, de la Roza-Delgado B, González A, Soldado A, Rodriguez ML, Peláez M, Vicente F (2011) Effect of feeding system on unsaturated fatty acid level in milk of dairy cows. Renew Agric Food Syst 26(3):224–229

    Article  Google Scholar 

  • Palmquist DL, Jenkins TC (2003) Challenges with fats and fatty acid methods. J Anim Sci 81:3250–3254

    CAS  Google Scholar 

  • SAS (1999) SAS/STATTM user’s guide. Statistical Analysis System Institute Inc, Cary

    Google Scholar 

  • Söderholm SL, Damm M, Kappe CO (2010) Microwave-assisted derivatization procedures for gas chromatography/mass spectrometry analysis. Mol Divers 14:869–888

    Article  Google Scholar 

  • Sparr C, Björklund E (2000) Analytical-scale microwave-assisted extraction. J Chromatogr A 902:227–250

    Article  Google Scholar 

Download references

Acknowledgments

The authors wish to thank the laboratory staff of the Department of Animal Nutrition Grassland and Forages at the Regional Institute of Agro-food, Research and Development (SERIDA) for their assistance, especially to Alejandro Argamentería and Alfonso Carballal, for their invaluable help in the statistical analysis of the experimental results. This study was financially supported by the Spanish Project RTA2012-00063-C02-00 from the INIA and PC10-54 from the Asturias Regional Project and European Regional Development Fund (ERDF). The authors also want to thank the Spanish Reference Laboratory for milk and milk products (EA Search Facility, no. 517/LE1040) for providing butter reference material.

Compliance with Ethics Requirements

This article does not contain any studies with human or animal subjects

Conflict of Interest

The authors have no financial relationship with the organization that sponsored the research. All authors declare that they have no conflict of interest.

Author information

Authors and Affiliations

Authors

Corresponding author

Correspondence to Begoña de la Roza-Delgado.

Rights and permissions

Reprints and permissions

About this article

Check for updates. Verify currency and authenticity via CrossMark

Cite this article

González-Arrojo, A., Soldado, A., Vicente, F. et al. Microwave-Assisted Methodology Feasibility for One-Step Extraction and Transmethylation of Fatty Acids in Milk for GC-Mass Spectrometry. Food Anal. Methods 8, 2250–2260 (2015). https://doi.org/10.1007/s12161-015-0108-8

Download citation

  • Received:

  • Accepted:

  • Published:

  • Issue Date:

  • DOI: https://doi.org/10.1007/s12161-015-0108-8

Keywords

Profiles

  1. Ana Soldado