Rapid analyses of oil and fat content in agri-food
products using continuous wave free precession
time domain NMR
†
L. A. Colnago,
a
* R. B. V. Azeredo,
b
A. Marchi Netto,
c
F. D. Andrade
d
and
T. Venâncio
e
Time-domain nuclear magnetic resonance (TD-NMR) is one of the most popular solutions for quality control in the food
industry. Despite the recognized success of TD-NMR in quality control and quality assurance, the speed by which samples
can be characterized by TD-NMR techniques is still a concern, primarily when considering online or high-throughput
applications. Therefore, to enhance the speed of TD-NMR analysis, we developed rapid methods based on steady-state free
precession of nuclear spins, which we denoted continuous wave free precession (CWFP). CWFP substantially increases the
sensitivity of TD-NMR compared with free induction decay or spin-echo detection, which are traditionally used. The objective
of this paper was to present the physical background of CWFP and review its recent developments and applications in fat and
oil quantifications in agri-food products. Copyright © 2012 John Wiley & Sons, Ltd.
Keywords: continuous wave free precession; steady-state free precession; time domain NMR; oil and fat; agri-food products; online
NMR; high-throughput NMR
Introduction
Most of the traditional methods for food analysis are time consum-
ing, destructive, and/or performed in multiple steps. Therefore,
several investigators have reported the application of spectroscopic
methods to complement or even replace the traditional methods
used in food quality control and assurance (QC/QA).
[1–6]
Among all
of the spectroscopic methods, time domain nuclear magnetic
resonance (TD-NMR) has been the most popular solution for quality
control in the industrial sector.
[1–3,7,8]
Time domain nuclear magnetic
resonance also is known as low-field NMR or low-resolution NMR.
The analyses are primarily performed on low-cost benchtop
spectrometers with permanent magnets. The low intensity of the
magnetic field and the lack of magnetic field homogeneity do
not allow the detection of chemical shift, which eliminates the
application of the Fourier transform. In general, TD quantifica-
tions are based on the analysis of the amplitude (absolute or
relative) of the free induction decay and/or spin-echo.
Importantly, both relaxometry and diffusometry, which also
are part of the TD-NMR routine experiments, are inserted as
filters in a specific pulse sequence
[9]
or performed as an
independent measurement.
[10]
Nuclear magnetic resonance was first used to measure oil
content in an agri-food product (i.e. corn seeds) in 1963.
[11]
This
analysis was performed with a continuous wave NMR spectrom-
eter. The advent of pulsed TD-NMR instruments 40 years ago
initiated efforts to develop a small bench-top NMR analyzer that
was dedicated to animal and vegetable oil and fat analysis.
[1]
Today, TD-NMR is an off-the-shelf NMR solution that is recog-
nized as a standard international method for several agencies.
[12–17]
Despite its recognized success in the QC/QA context, the
speed by which samples can be characterized by TD-NMR
techniques is still a concern, primarily when considering online
or high-throughput applications. Therefore, to enhance the
speed of TD-NMR analysis, several authors have been develop-
ing instrumentation and applications of online NMR for analysis
of agri-food products such as avocado, cherry, lemon, orange,
olive, and pear.
[18–22]
We have been developing online NMR method for measur-
ing oil/fat content and quality based on steady-state free
precession (SSFP) of nuclear spins, denoted continuous wave
free precession (CWFP).
[23–29]
Continuous wave free precession
has several interesting features, including a substantially
increased sensitivity
[23,24]
compared with detection of free
induction decay FID or spin-echo, which are traditionally used
in the TD-NMR context.
* Correspondence to: Luiz Alberto Colnago, Embrapa Instrumentação, Rua XV de
Novembro 1452, São Carlos, SP, Brazil 13560–970. E-mail: colnago@cnpdia.
embrapa.br
a Embrapa Instrumentação, São Carlos, São Paulo, Brazil
b Instituto de Química, Universidade Federal Fluminense, Niterói, Rio de Janeiro,
Brazil
c Instituto de Física de São Carlos, Universidade de São Paulo, São Carlos, São
Paulo, Brazil
d Instituto de Química de São Carlos, Universidade de São Paulo, São Carlos, São
Paulo, Brazil
e Departamento de Química, Universidade Federal de São Carlos, São Carlos,
São Paulo, Brazil
†
This article is published in Magnetic Resonance in Chemistry as a special issue
on Magnetic Resonance in Food-Dealing with Complex Systems, edited by
Belton and Capozzi.
Magn. Reson. Chem. 2011, 49, S113–S120 Copyright © 2012 John Wiley & Sons, Ltd.
Special Issue Review
Received: 3 June 2011 Revised: 2 September 2011 Accepted: 21 September 2011 Published online in Wiley Online Library
(wileyonlinelibrary.com) DOI 10.1002/mrc.2841
S113