Multicomponent analysis of encapsulated marine oil supplements using high-resolution 1H and 13C NMR techniques

Siddiqui, Navaede; Sim, Julia; Silwood, Christopher J.L.; Toms, Harold; Iles, Richard A.; Grootveld, Martin

doi:10.1194/jlr.d300017-jlr200

Cited by 76 publications

(73 citation statements)

References 39 publications

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“…In this region, intense signals were observed between d 132.0 and 127.0 ppm, which were attributed to the n-3C atoms in polyunsaturated fatty acids. The greater concentration of n-3 fatty acids in E 6 (22.1% of total fatty acids) was reflected in the greater intensity signals at d 129.72 and 130.456 ppm that were assigned to the two olefinic n-3 carbons [28,24]. Due to the greater concentration of EPA, which contain five non-conjugated double bounds, the majority of the high intensity olefinic resonances were observed at d 127.8-129.1 ppm, which was originated from this fatty acid.…”

Section: H-nmr Analysismentioning

confidence: 99%

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Cooking and pressing is an effective and eco‐friendly technique for obtaining high quality oil from Sardinella longiceps

Chakraborty

Joseph

2015

Euro J Lipid Sci & Tech

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The conventional Bligh and Dyer method of extracting oil from the edible tissues of Sardinella longiceps was compared with different eco-friendly methodologies using 40% ethanol, 95% ethanol, distilled water, and cooking followed by pressing, as well as cooking followed by the Bligh and Dyer method. Among the different methods studied, cooking followed by pressing showed a beneficial effect on the quality of the oil as evidenced by reduced saponification (209.8 mg KOH/g), peroxide (11.88 meqO 2 / kg), para-anisidine (16.2), total oxidation (39.96), and TBARS (6.18 MDAEQ/kg) values. A comparable lipid yield (8.3%) with that of the Bligh and Dyer method was attained through the cooking and pressing method. The greater induction time (0.13 h) indicated better oxidative stability of cooked and pressed oil as compared to the oil obtained using other methods. The fish oil obtained by cooking followed by pressing has been demonstrated to yield comparable amounts of eicosapentaenoic acid, docosahexaenoic acid, and total polyunsaturated fatty acid contents when compared to the Bligh and Dyer method. These results demonstrated the effectiveness of the cooking and pressing technique for obtaining the best quality oil from Sardinella longiceps. The oil obtained by the cooking and pressing mode was characterized by FTIR and NMR experiments.Practical applications: The advantages of the method involving cooking followed by pressing as compared to the traditional Bligh and Dyer method were the absence of toxic solvents along with reduced cost and labor requirements. In addition, no chemical wastes were generated in this technique. The cooking followed by pressing method has been demonstrated to improve the nutritive value and oxidative stability of the crude fish oil as compared to the new eco-friendly methods studied and the traditional method. The utilities of FTIR and NMR analyses as new analytical tools for analyzing the chemistry of fish oil have been demonstrated in the present study. This study is significant for the extraction of greater quality marine fish oil for use in pharmaceutical industries.

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Section: H-nmr Analysismentioning

confidence: 99%

“…4A and B). Peak assignments were performed with the aid of literature data [24,25], and by recording spectra of standard compounds. The signals at d 0.85-0.92 ppm (Fig.…”

Section: H-nmr Analysismentioning

confidence: 99%

Cooking and pressing is an effective and eco‐friendly technique for obtaining high quality oil from Sardinella longiceps

Chakraborty

Joseph

2015

Euro J Lipid Sci & Tech

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“…Detailed chemical composition of algae biomass is essential to understand the chemistry of neutral and polar lipids to explore their biodiesel and high value product potential as well as help in the prediction of quality, yield and physio-chemical properties of the algae derived fuels. Therefore, analytical methods based on NMR [7,8,14,24,[29][30][31][32][33][34][35][36][37][38][39] , GC/GC-MS [7,8,40,41] , IR [24,42] and HPLC [43] techniques are used to characterize and determine the neutral lipids content and their fatty acids composition of the algal oils. The importance of solvent polarity in the extraction of lipids and their composition, fatty acid profile, and yield has been reported from critical analyses of extracted oils obtained by different solvents by GC-MS and gravimetric methods [21] .…”

Section: Introductionmentioning

confidence: 99%

comparison of oil extraction methods for algae by NMR and Chromatographic techniques

Sarpal¹,

Sharma²,

Scott³

et al. 2016

JABST

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The present study focuses on identification and compositional characterization of neutral (tri acyl glycerides, TAG; free fatty acids, FFA) and polar (glyco/ glycerophospho) lipids, and fatty acid chains constituting these lipids in the cyclohexane, dichloromethane and methanol extracts or algal oils of microalgae biomasses. Algal oils were generated by step wise Accelerated Solvent and Soxhlet extraction methods from six microalgae biomasses (Scenedesmus dimorph, Chlorella vulgaris, Spirulina, SD Flakes, Cyanothece and Chlamydomonas) obtained from commercial sources. The analytical protocol developed based on NMR (300 & 400 MHz)( 1 H & 13 C), IR, GPC, GC-FID and GC-MS techniques has provided authentic quantitative information about the nature of neutral lipids, polar lipids, fatty acid profiles, oxylipins (oxo fatty acids) and hydrocarbons present in the extracts. The analyses of fractions generated by silica column chromatographic separation of solvent extracts have facilitated demarcation of 1 H NMR chemical shift regions of functional groups corresponding to neutral and polar lipids. Specifically, α (n-3) and γ (n-6) C18:3 were differentiated in the Spirulina by critical examination of 1 H NMR spectral features of algal oils from various biomasses. The comparative results by different analytical techniques have shown that newly developed methods based on 1 H NMR techniques can provide direct and rapid quantitative results of neutral lipids components including poly unsaturated fatty acid/ester (PUFA/PUFE) in the algal oils without prior sample treatment. The neutral lipids results obtained by NMR and GPC show good agreement as compared by linear regression analyses. The results showed that nature and contents of neutral lipids, and fatty acids profile in the extracts were dependent upon the methods of extraction and the polarity index of solvent used for extraction, and specific to types of algae strains. The application of NMR and IR techniques enabled assessment of the solvent extraction efficiency towards extraction of neutral and polar lipids including types of fatty acids constituting these lipids.

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“…The combination of 1H and 13C spectra permitted the detailed analysis of components, including sn-1 monoacylglycerols, sn-1,2-and sn-1,3-diacylglycerol adducts, and other minor components, such as trans-fatty acids, free glycerol and cholesterol, and added vitamins A and E and synthetic compounds, such as ethyl docosahexaenoate or eicosopentaenoate. The identity of each compound was confirmed using 2D COSY [63].…”

Section: Metabolomic Profiling Using 13c Nmrmentioning

confidence: 99%

1H and 13C NMR for the Profiling of Natural Product Extracts: Theory and Applications

Dayrit¹,

Dios²

2017

Spectroscopic Analyses - Developments and Applications

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Nuclear magnetic resonance (NMR) spectroscopy and mass spectrometry (MS) are the principal methods of metabolomics, the branch of '-omics' that deals with small molecules. Although MS is gaining popularity in metabolomics, NMR enjoys a number of key advantages because it is nondestructive, unbiased, quantitative, does not require separation or derivatization, and is amenable to compounds that are difficult to analyze by gas chromatography-mass spectrometry (GC-MS) and liquid chromatography-mass spectrometry (LC-MS). There are two general approaches to the use of NMR for profiling studies: an untargeted approach, which uses chemometric analysis; and a targeted approach, which aims to quantify known compounds in the extract. These approaches, however, are not mutually exclusive and will likely converge in the future. This paper will describe the basic theoretical principles that should be considered to develop NMR into a standard quantitative method. Although 1H NMR is more sensitive, 13C NMR spectra are simpler with less overlapping signals and are less affected by different magnetic field strengths. Various applications of 1H and 13C NMR for the profiling of natural products are described. The use of two-dimensional 1H NMR has been used to overcome problems of spectral overlap. The standardization of the NMR protocol will make it a more useful tool for the profiling of natural products extracts.

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Multicomponent analysis of encapsulated marine oil supplements using high-resolution 1H and 13C NMR techniques

Cited by 76 publications

References 39 publications

Cooking and pressing is an effective and eco‐friendly technique for obtaining high quality oil from Sardinella longiceps

Cooking and pressing is an effective and eco‐friendly technique for obtaining high quality oil from Sardinella longiceps

comparison of oil extraction methods for algae by NMR and Chromatographic techniques

1H and 13C NMR for the Profiling of Natural Product Extracts: Theory and Applications

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