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Application of a Novel, Heated, Nine-Reflection ATR Crystal and a Portable FTIR Spectrometer to the Rapid Determination of Total Trans Fat

Mossoba, Magdi M., Kramer, John K. G., Azizian, Hormoz, Kraft, Jana, Delmonte, Pierluigi, Kia, Ali-Reza Fardin, Bueso, Francisco J., Rader, Jeanne I., Lee, Jung K.
journal of the American Oil Chemists' Society 2012 v.89 no.3 pp. 419-429
Fourier transform infrared spectroscopy, absorption, compliance, deformation, instrumentation, lipid content, trans fatty acids, United States
Since trans fat labeling requirements became mandatory in the US and many other countries, there has been a need for rapid and accurate analytical methodologies that can facilitate compliance with the various regulations. The determination of total trans fatty acids by mid-infrared (IR) spectroscopy is a widely used procedure that was standardized and validated as AOCS Official Method Cd 14e-09 (negative second derivative infrared spectroscopic method for the rapid (5 min) determination of total isolated trans fat) in 2009. The C–H out-of-plane deformation mid-IR band observed at 966 cm⁻¹ is uniquely characteristic of isolated (non-conjugated) double bonds with trans configuration. AOCS Official Method Cd 14e-09, the most recent attenuated total reflection-Fourier transform IR (ATR-FTIR) official method, entails the measurement of the height of the negative second derivative of the trans absorption band. In the present study, the performance of a novel, portable FTIR system equipped with a heated 9-bounce diamond ATR crystal was evaluated and compared to that of a conventional benchtop single-bounce ATR-FTIR spectrometer. The introduction of the 9-bounce diamond ATR crystal resulted in the lowering of the limit of quantification of trans fat, as a percentage of the total fat, from approximately 2 to 0.34%. The data collected from accurately weighed gravimetric standards and 28 unknown test samples ranging in trans fat content from about 0.5 to 54%, as a percentage of the total fat, indicated that this IR official method and the use of the new 9-bounce portable ATR-FTIR instrumentation could lead to a five-fold enhancement in sensitivity relative to single-bounce systems. Implementing these changes would facilitate regulatory compliance and verification of fat and oil samples for trans fat content in the US and other countries, since all of the published regulations (e.g., “0 g trans fat per serving”) have levels of trans fat, as percentage of total fat, that exceed 0.34%.