Rapid quantitation of fish oil fatty acids and their ethyl esters by FT‐NIR models

Azizian, Hormoz; Kramer, J. K. G.; Ehler, Shannon; Curtis, Jonathan M.

doi:10.1002/ejlt.200900186

Cited by 34 publications

(35 citation statements)

References 29 publications

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“…Many of the unsaturated FA with one or more trans double bonds coelute with their all-cis isomers when separated on PEG-coated columns [10], which could lead to overestimation of the all-cis LC n-3 PUFA content of fish products. This observation was recently confirmed when Fourier transform near-infrared (FT-NIR) spectroscopy was evaluated as an alternative method for LC n-3 PUFA determination [20]. FT-NIR quantification based on calibrated data acquired with a PEG column overestimated the amount of the all-cis LC n-3 PUFA compared with FT-NIR quantification based on calibration data obtained by use of a 100-m highly polar CPS column.…”

Section: Introductionmentioning

confidence: 83%

“…This would explain why Sébédio et al [11] found only geometric isomers of LC highly unsaturated PUFA in deep fried mackerel by use of a 30-m Supelcowax-10 column, the same GC column we used. We recently evaluated FT-NIR for quantification of FA in fish oil preparations enriched with EPA and DHA [20]. We observed that the amount of the all-cis highly unsaturated FA contained in these oils was significantly overestimated when a 30-m PEG FAMEWAX column was used for calibration of the FT-NIR spectrometer, rather than when a 100-m CP Sil 88 column was used.…”

Section: Discussionmentioning

confidence: 99%

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Comparison of Separations of Fatty Acids from Fish Products Using a 30‐m Supelcowax‐10 and a 100‐m SP‐2560 Column

Santercole¹,

Delmonte

Kramer

2012

Lipids

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Commercial fish oils and foods containing fish may contain trans and/or isomerized fatty acids (FA) produced during processing or as part of prepared foods. The current American Oil Chemists' Society (AOCS) official method for marine oils (method Ce 1i-07) is based on separation by use of poly(ethylene glycol) (PEG) columns, for example Supelcowax-10 or equivalent, which do not resolve most unsaturated FA geometric isomers. Highly polar 100-m cyanopropyl siloxane (CPS) columns, for example SP-2560 and CP Sil 88 are recommended for separation of geometric FA isomers. Complementary separations were achieved by use of two different elution temperature programs with the same CPS column. This study is the first direct comparison of the separations achieved by use of 30-m Supelcowax-10 and 100-m SP-2560 columns for fatty acid methyl esters (FAME) prepared from the same fish oil and fish muscle sample. To simplify the identification of the FA in these fish samples, FA were fractionated on the basis of the number and type of double bonds by silver-ion solid-phase extraction (Ag⁺-SPE) before GC analysis. The results showed that a combination of the three GC separations was necessary to resolve and identify most of the unsaturated FA, FA isomers, and other components of fish products, for example phytanic and phytenic acids. Equivalent chain length (ECL) values of most FAME in fish were calculated from the separations achieved by use of both GC columns; the values obtained were shown to be consistent with previously reported values for the Supelcowax-10 column. ECL values were also calculated for the FA separated on the SP-2560 column. The calculated ECL values were equally valid under isothermal and temperature-programmed elution GC conditions, and were valuable for confirmation of the identity of several unsaturated FAME in the fish samples. When analyzing commercially prepared fish foods, deodorized marine oils, or foods fortified with marine oils it is strongly recommended that quantitative data acquired by use of PEG columns is complemented with data obtained from separations using highly polar CPS columns.

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Section: Introductionmentioning

confidence: 83%

Section: Discussionmentioning

confidence: 99%

Comparison of Separations of Fatty Acids from Fish Products Using a 30‐m Supelcowax‐10 and a 100‐m SP‐2560 Column

Santercole¹,

Delmonte

Kramer

2012

Lipids

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“…Six replicate absorption spectra were measured for each test portion. These spectra were subsequently used to generate an average spectrum and in the development of PLS1 calibration models for the determination of FT-NIR index values, FA composition [28][29][30], and adulterant type and concentration in spiked EVOO samples. Various pre-processing steps were carried out as described below.…”

Section: Methodsmentioning

confidence: 99%

“…The previously developed PLS1 calibration models to determine the FA composition of oils were based on observed FT-NIR spectra and used accurate GC determinations as primary reference [28][29][30]. All FA calibration models were updated and optimized for the determination of FA markers in EVOO.…”

Section: Development Of Pls1 Calibration Models For Rapid Determinatimentioning

confidence: 99%

“…Factors that affected the intensity of the absorption band near 5280 cm −1 were also investigated. Then using the same FT-NIR spectra and the pre-developed PLS1 calibration models that were optimized in the present study (NIR Technologies Inc.), the fatty acid (FA) composition [28][29][30] of the oils investigated was obtained. Additionally, FT-NIR spectra and PLS1 calibration models generated for gravimetric mixtures of EVOO spiked with nine different suspected adulterant oils were used to predict the nature and amount of an adulterant in test samples of EVOO.…”

Section: Introductionmentioning

confidence: 99%

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Novel, Rapid Identification, and Quantification of Adulterants in Extra Virgin Olive Oil Using Near‐Infrared Spectroscopy and Chemometrics

Azizian¹,

Mossoba

Fardin‐Kia

et al. 2015

Lipids

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116

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A new, rapid Fourier transform near infrared (FT-NIR) spectroscopic procedure is described to screen for the authenticity of extra virgin olive oils (EVOO) and to determine the kind and amount of an adulterant in EVOO. To screen EVOO, a partial least squares (PLS1) calibration model was developed to estimate a newly created FT-NIR index based mainly on the relative intensities of two unique carbonyl overtone absorptions in the FT-NIR spectra of EVOO and other mixtures attributed to volatile (5280 cm(-1)) and non-volatile (5180 cm(-1)) components. Spectra were also used to predict the fatty acid (FA) composition of EVOO or samples spiked with an adulterant using previously developed PLS1 calibration models. Some adulterated mixtures could be identified provided the FA profile was sufficiently different from those of EVOO. To identify the type and determine the quantity of an adulterant, gravimetric mixtures were prepared by spiking EVOO with different concentrations of each adulterant. Based on FT-NIR spectra, four PLS1 calibration models were developed for four specific groups of adulterants, each with a characteristic FA composition. Using these different PLS1 calibration models for prediction, plots of predicted vs. gravimetric concentrations of an adulterant in EVOO yielded linear regression functions with four unique sets of slopes, one for each group of adulterants. Four corresponding slope rules were defined that allowed for the determination of the nature and concentration of an adulterant in EVOO products by applying these four calibration models. The standard addition technique was used for confirmation.

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Progression to Fatty Acid Profiling of Edible Fats and Oils Using Vibrational Spectroscopy

Azizian¹,

Kramer²,

Mossoba³

2001

Handbook of Vibrational Spectroscopy

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The contributions of vibrational spectroscopy (FT‐mid‐IR, FT‐Raman, and FT‐NIR) in the analyses of edible fats and oils have been reviewed. The major contributions of FT‐mid‐IR and FT‐Raman have been in structural analysis and for quantitative determination of total unsaturation, trans fat and conjugated linoleic acid (CLA). The current method of choice for fatty acid (FA) determination is GC; however it is time consuming, uses solvents, and FA must be converted to methyl esters before analysis. A rapid spectroscopic method is needed to determine both the FA composition and total trans content to meet current regulatory compliance for labeling purposes. FT‐mid‐IR and FT‐Raman lack the specificity of GC for FA determinations, while FT‐NIR is able to determine the concentration of all FAs using predeveloped spectral models based on accurate GC results. The biological activity of different FA isomers differs; some are harmful while others may have health benefits. This applies specifically to the CLA and trans isomers, since only rumenic acid (9 c 11 t ‐CLA) and its precursor vaccenic acid (11 t ‐18:1) have reported health benefits. Therefore, the current trans regulation may need to be revised to reflect the reality of the scientific evidence. The FT‐NIR method is well equipped to selectively exclude or include specific FAs for labeling purposes because it determines the complete FA composition.

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Rapid quantitation of fish oil fatty acids and their ethyl esters by FT‐NIR models

Cited by 34 publications

References 29 publications

Comparison of Separations of Fatty Acids from Fish Products Using a 30‐m Supelcowax‐10 and a 100‐m SP‐2560 Column

Comparison of Separations of Fatty Acids from Fish Products Using a 30‐m Supelcowax‐10 and a 100‐m SP‐2560 Column

Novel, Rapid Identification, and Quantification of Adulterants in Extra Virgin Olive Oil Using Near‐Infrared Spectroscopy and Chemometrics

Progression to Fatty Acid Profiling of Edible Fats and Oils Using Vibrational Spectroscopy

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