Determination of <i>trans</i> fatty acids in hydrogenated vegetable oils by attenuated total reflection infrared spectroscopy: Two limited collaborative studies

Adam, Michael J.; Chew, Michael Yit Lin; Wasserman, S.; McCollum, A.; McDonald, Roderick P.; Mossoba, Magdi M.

doi:10.1007/s11746-998-0052-5

Cited by 16 publications

(12 citation statements)

References 12 publications

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“…This modified IR procedure (6) was also rapid (5 min) because an attenuated total reflection (ATR) liquid cell (capacity 1.5-2 mL) was used that required neither weighing nor quantitative dilution of neat melted fat test samples in any solvent. By using a single-bounce horizontal ATR cell with 50 µL capacity, this ATR IR procedure was optimized and applied to the determination of total trans fatty acids in commercial food products (11), validated in two limited collaborative studies (12), and adopted as Recommended Practice AOCS Cd 14d-97 (13). Attempts were abandoned to use a single-µL ATR cell for the quantitation of trans fatty acids in biological matrices (14,15) due to spectral interferences from conjugated fatty acids.…”

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Comparison of attenuated total reflection infrared spectroscopy to capillary gas chromatography for trans fatty acid determination

Adam¹,

Mossoba

Dawson

et al. 1999

J Americ Oil Chem Soc

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Gas chromatography (GC) has been a standard analytical tool in lipid chemistry. The rapid attenuated total reflection (ATR) infrared (IR) American Oil Chemists' Society (AOCS) Recommended Practice (Cd 14d-97) was compared to the capillary GC AOCS Recommended Practice (Ce 1f-97) that was optimized to accurately determine total trans fatty acids on highly polar stationary phases. This comparative evaluation was validated in an independent laboratory. These procedures were used to quantitate the total trans fatty acid levels in partially hydrogenated vegetable oils, measured as neat (without solvent) triacylglycerols (TAG) by ATR and as fatty acid methyl ester (FAME) derivatives by capillary GC. Unlike FAME, TAG determination by ATR required no derivatization, but samples had to be melted prior to measurement. Five blind replicates for each of three accuracy standards and three test samples were analyzed by each technique. The GC and ATR determinations were in good agreement. Accuracy was generally high. The ratios of ATR mean trans values (reported as percentage of total TAG) to the true values (based on the amount of trielaidin added gravimetrically) were 0.89, 0.98, and 1.02 for accuracy standards having about 1, 10, and 40% trans levels. The corresponding GC values, determined as percentage of total FAME, were 0.98, 0.99 and 1.04. The ratios of mean trans values determined by these techniques were ATR/GC 0.85, 1.04, and 1.01 for test samples having trans levels of about 0.7, 8, and 38%, respectively. The optimized GC procedure also minimized the expected low bias in trans values due to GC peak overlap found with the GC Official Method Ce 1c-89. Satisfactory repeatability and reproducibility were obtained by both ATR and GC.For several decades analytical methods, such as gas chromatography (GC) (1) and infrared (IR) spectroscopy (2,3), for the determination of total trans fatty acids in partially hydrogenated vegetable oils have each been widely used (4) and repeatedly modified in order to improve accuracy (5,6). A recent publication by Duchateau et al. (5) detailed optimized capillary GC separations on highly polar stationary phases for the accurate determination of trans fatty acids in partially hydrogenated vegetable oils and in refined (deodorized or stripped) oils. This procedure was adopted by the American Oil Chemists' Society (AOCS) as Official Method AOCS Ce 1f-96 (7). The GC Official Method AOCS Ce 1c-89 (1) for partially hydrogenated vegetable oils underestimates some trans C 18 monoene (18:1) positional isomers in favor of cis 18:1 isomers, with which they overlap. Two relatively minor peaks attributed to the trans-12 and trans-13 plus trans-14 18:1 isomers were resolved by the optimized GC procedure (5), and this reportedly improved the accuracy of the GC determination. These two minor peaks (labeled "valley peaks") emerged between those of the major trans 18:1 isomers and the intense cis-9 18:1 peak. In refined vegetable oils monotrans 18:2 and 18:3 isomers occur at levels that can reach 1-3% of tot...

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Comparison of attenuated total reflection infrared spectroscopy to capillary gas chromatography for trans fatty acid determination

Adam¹,

Mossoba

Dawson

et al. 1999

J Americ Oil Chem Soc

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“…Studies assessed accuracy, repeatability and reproducibility in the analysis of trielaidin and methyl elaidate standards, refined oil and partially hydrogenated vegetable oils (PHVO), and oils spiked with trielaidin [35,36]. Repeatability and reproducibility are suitable for middle or high TFA levels, but decrease when TFA amounts approach the quantification limit (1% TFA as % total FA).…”

Section: Atr-ftir Spectrometrymentioning

confidence: 99%

Analytical methods for determination of trans fatty acid content in food

Juanéda¹,

Ledoux

Sébédio

2007

Euro J Lipid Sci & Tech

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Adequate analytical tools are required for labelling food products for trans fatty acid (TFA) contents. The choice of the fatty acid (FA) derivatisation is a crucial step in obtaining good results, in particular with short-chain and conjugated FA. Several gas chromatographic and infrared spectrophometric methods have been developed for analysing TFA in foods, some of which have been validated as official methods after collaborative studies. Complete analysis of total FA often requires the use of complementary high-performance liquid chromatography methods. This paper reviews the analytical methods developed for identifying and quantifying TFA in foods and presents the official methods of analysis. Neither of these analytical methods enables a TFA naturally occurring in basic food to be distinguished from a TFA formed during an industrial process.

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“…By using this 50-µL cell, two collaborative studies were conducted (8) in each of five laboratories on neat triacylglycerols (TAG) and the corresponding neat FAME derivatives. The lower limit of trans quantitation was about 1% of total fat.…”

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“…The lower limit of trans quantitation was about 1% of total fat. Because it was demonstrated that the "ratioing" and ATR procedure was an acceptable alternative for the IR determination of the total trans fatty acid content (6)(7)(8)(9), it was adopted as Recommended Practice Cd 14d-96 by AOCS in 1996 (10). Recently, it was used by Sedman et al (11) as a reference method to validate a proposed transmission IR procedure.…”

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“…The ATR procedure is rapid because it requires little or no preparation of the test sample, and requires only about 5 min for spectroscopic signal averaging, band area integration, and calculation of the trans content from a linear regression equation. It also requires no derivatization of fats and oils to FAME (8). Recently, an attempt was made to apply the standard addition technique to enhance the accuracy of the attenuated total reflection Fourier transform infrared (ATR-FTIR) determination (12).…”

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Rapid determination of total Trans fat content by attenuated total reflection infrared spectroscopy: An international collaborative study

Adam¹,

Mossoba

Lee

2000

J Americ Oil Chem Soc

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Interest in trans fat labeling has prompted efforts to develop new, more efficient methods for rapidly and accurately determining trans fat content in foods. The lower limit of quantitation, 5% trans fat (as percent of total fat), of transmission infrared official methods, such as AOAC 994.14 and 965.34, for total isolated trans fatty acids is too high to be generally useful for the determination of low levels of trans fats in foods. A novel and rapid (5 min) attenuated total reflection Fourier transform infrared (ATR-FTIR) spectroscopic procedure was recently developed and applied to food products. This procedure was voted official method AOCS Cd 14d-99 by the American Oil Chemists' Society in 1999 after testing in a 12-laboratory international collaborative study. The results of this study are described in this paper. Analytical ATR-FTIR results exhibited high accuracy in the range investigated, 1-40% trans; results tended to have <2% high bias relative to the gravimetrically determined values. The precision of this internal reflection method was found to be superior to those of transmission infrared official methods. It is recommended that the applicability of the ATR-FTIR method be limited to trans levels of >1% (as percent of total fat).

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Determination of trans fatty acids in hydrogenated vegetable oils by attenuated total reflection infrared spectroscopy: Two limited collaborative studies

Cited by 16 publications

References 12 publications

Comparison of attenuated total reflection infrared spectroscopy to capillary gas chromatography for trans fatty acid determination

Comparison of attenuated total reflection infrared spectroscopy to capillary gas chromatography for trans fatty acid determination

Analytical methods for determination of trans fatty acid content in food

Rapid determination of total Trans fat content by attenuated total reflection infrared spectroscopy: An international collaborative study

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