Food Analytical Methods

, Volume 12, Issue 4, pp 991–997 | Cite as

Quantitative Determination of Fatty Acid Compositions in Edible Oils Using J-Selective 13C QDEPT

  • Yunyan Li
  • Wenping Mao
  • Chaoyang Liu
  • Xu ZhangEmail author
  • Junfeng WangEmail author


We propose a J-selective quantitative distortionless enhancement by polarization transfer (J-selective QDEPT) 13C NMR method with enhanced sensitivity for accurate determination of the fatty acid compositions of edible oils. The J-selective QDEPT protocol is developed by targeted optimization of the known Q-DEPT+ experiment. Based on the one-bond C-H J-coupling constants (1JCH) which can be measured with the heteronuclear two-dimensional J-resolved 13C NMR spectrum, it is possible to optimize the polarization transfer delay Δ and the reading pulse angle , thus enabling the QDEPT experiment further enhancing 13C resonance signals which have narrow 1JCH ranges over the traditional untargeted Q-DEPT. For edible oil applications, it is demonstrated that this procedure brings a 2.2 enhancement factor against 1.3 of the traditional untargeted Q-DEPT compared to the standard inverse-gated 13C experiment, even with a shorter relaxation delay for the two QDEPT experiments. Another advantage of J-selective QDEPT is that a smaller number of quantitative scans are needed to reach a uniform enhancement for different CHn (n = 1, 2, 3) groups. These features of the J-selective QDEPT are particularly attractive for batch analysis in the food industry.


Quantitative 13C NMR Sensitivity enhancement J-selective QDEPT Fatty acid Edible oil 



The authors would like to thank the Steady High Magnetic Field Facilities (High Magnetic Field Laboratory, Chinese Academy of Sciences, Hefei, China) for performing the NMR experiments.


This work was supported by the Ministry of Science and Technology of China (grant nos. 2016YFA0400901 and 2017YFA0505400), the National Natural Science Foundation of China (grant nos. U1532269 and 21675170), and the Major/Innovative Program of Development Foundation of Hefei Center for Physical Science and Technology (grant no. 2017FXZY004).

Compliance with Ethical Standards

Conflict of Interest

Yunyan Li declares that she has no conflict of interest. Wenping Mao declares that he has no conflict of interest. Chaoyang Liu declares that he has no conflict of interest. Xu Zhang declares that he has no conflict of interest. Junfeng Wang declares that he has no conflict of interest.

Ethical Approval

This article does not contain any studies with human participants or animals performed by any of the authors.

Informed Consent

Not applicable.

Supplementary material

12161_2019_1432_MOESM1_ESM.docx (166 kb)
ESM 1 (DOCX 165 kb)


  1. Castejon D, Mateos-Aparicio I, Molero MD, Cambero MI, Herrera A (2014) Evaluation and optimization of the analysis of fatty acid types in edible oils by H-1-NMR. Food Anal Methods 7:1285–1297. CrossRefGoogle Scholar
  2. Castejon D, Fricke P, Cambero MI, Herrera A (2016) Automatic H-1-NMR screening of fatty acid composition in edible oils. Nutrients 8:93. CrossRefGoogle Scholar
  3. Dugo G, Rotondo A, Mallamace D, Cicero N, Salvo A, Rotondo E, Corsaro C (2015) Enhanced detection of aldehydes in extra-virgin olive oil by means of band selective NMR spectroscopy. Phys A 420:258–264. CrossRefGoogle Scholar
  4. Fernandes JLN, de Souza ROMA, Azeredo RBD (2012) 13C NMR quantification of mono and diacylglycerols obtained through the solvent-free lipase-catalyzed esterification of saturated fatty acids. Magn Reson Chem 50:424–428. CrossRefGoogle Scholar
  5. Hammad SS, Jones PJ (2017) Dietary fatty acid composition modulates obesity and interacts with obesity-related genes. Lipids 52:803–822. CrossRefGoogle Scholar
  6. Hatzakis E, Dagounakis G, Agiomyrgianaki A, Dais P (2010) A facile NMR method for the quantification of total, free and esterified sterols in virgin olive oil. Food Chem 122:346–352. CrossRefGoogle Scholar
  7. Henderson TJ (2004) Sensitivity-enhanced quantitative C-13 NMR spectroscopy via cancellation of 1JCH dependence in DEPT polarization transfers. J Am Chem Soc 126:3682–3683. CrossRefGoogle Scholar
  8. Hidalgo FJ, Zamora R (2003) Edible oil analysis by high-resolution nuclear magnetic resonance spectroscopy: recent advances and future perspectives. Trends Food Sci Technol 14:499–506. CrossRefGoogle Scholar
  9. Jiang B, Xiao M, Liu HL, Zhou ZM, Mao XA, Liu ML (2008) Optimized quantitative DEPT and quantitative POMMIE experiments for C-13 NMR. Anal Chem 80:8293–8298. CrossRefGoogle Scholar
  10. Lucas-Torres C, Perez A, Cabanas B, Moreno A (2014) Study by P-31 NMR spectroscopy of the triacylglycerol degradation processes in olive oil with different heat-transfer mechanisms. Food Chem 165:21–28. CrossRefGoogle Scholar
  11. Makela AV, Kilpelainen I, Heikkinen S (2010) Quantitative C-13 NMR spectroscopy using refocused constant-time INEPT, Q-INEPT-CT. J Magn Reson 204:124–130. CrossRefGoogle Scholar
  12. Mannina L, Sobolev AP (2011) High resolution NMR characterization of olive oils in terms of quality, authenticity and geographical origin. Magn Reson Chem 49:S3–S11. CrossRefGoogle Scholar
  13. Manu VS, Kumar A (2013) Fast and accurate quantification using genetic algorithm optimized H-1-C-13 refocused constant-time INEPT. J Magn Reson 234:106–111. CrossRefGoogle Scholar
  14. Merchak N, Silvestre V, Loquet D, Rizk T, Akoka S, Bejjani J (2017) A strategy for simultaneous determination of fatty acid composition, fatty acid position, and position-specific isotope contents in triacylglycerol matrices by C-13-NMR. Anal Bioanal Chem 409:307–315. CrossRefGoogle Scholar
  15. Merchak N, Rizk T, Silvestre V, Remaud GS, Bejjani J, Akoka S (2018) Olive oil characterization and classification by C-13 NMR with a polarization transfer technique: a comparison with gas chromatography and H-1 NMR. Food Chem 245:717–723. CrossRefGoogle Scholar
  16. Orsavova J, Misurcova L, Ambrozova J, Vicha R, Mlcek J (2015) Fatty acids composition of vegetable oils and its contribution to dietary energy intake and dependence of cardiovascular mortality on dietary intake of fatty acids. Int J Mol Sci 16:12871–12890. CrossRefGoogle Scholar
  17. Pelser C, Mondul AM, Hollenbeck AR, Park Y (2013) Dietary fat, fatty acids, and risk of prostate cancer in the NIH-AARP diet and health study. Cancer Epidemiol Biomark Prev 22:697–707. CrossRefGoogle Scholar
  18. Rotondo A, Salvo A, Gallo V, Rastrelli L, Dugo G (2017) Quick unreferenced NMR quantification of squalene in vegetable oils. Eur J Lipid Sci Technol 119:1–6. CrossRefGoogle Scholar
  19. Salvo A, Rotondo A, La Torre GL, Cicero N, Dugo G (2017) Determination of 1,2/1,3-diglycerides in Sicilian extra-virgin olive oils by 1H-NMR over a one-year storage period. Nat Prod Res 31:822–828. CrossRefGoogle Scholar
  20. Willett WC (2012) Dietary fats and coronary heart disease. J Intern Med 272:13–24. CrossRefGoogle Scholar

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© Springer Science+Business Media, LLC, part of Springer Nature 2019

Authors and Affiliations

  1. 1.High Magnetic Field LaboratoryChinese Academy of SciencesHefeiChina
  2. 2.Key Laboratory of High Magnetic Field and Ion Beam Physical BiologyChinese Academy of SciencesHefeiChina
  3. 3.Wuhan Center for Magnetic Resonance, State Key Laboratory of Magnetic Resonance and Atomic and Molecular Physics, Wuhan Institute of Physics and MathematicsChinese Academy of SciencesWuhanChina
  4. 4.Institute of Physical Science and Information TechnologyAnhui UniversityHefeiChina

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