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WO2015067834A1 - Procédé, dispositif et système de contrôle de la qualité des aliments - Google Patents

Procédé, dispositif et système de contrôle de la qualité des aliments Download PDF

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Publication number
WO2015067834A1
WO2015067834A1 PCT/ES2014/070825 ES2014070825W WO2015067834A1 WO 2015067834 A1 WO2015067834 A1 WO 2015067834A1 ES 2014070825 W ES2014070825 W ES 2014070825W WO 2015067834 A1 WO2015067834 A1 WO 2015067834A1
Authority
WO
WIPO (PCT)
Prior art keywords
sample
bioimpedance
spectrum
spectrometer
processing means
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Ceased
Application number
PCT/ES2014/070825
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English (en)
Spanish (es)
Inventor
Juan Francisco DUQUE CARRILLO
José Luís AUSÍN SÁNCHEZ
Javier RAMOS MAGANÉS
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
BIOBEE TECHNOLOGIES SL
Universidad de Extremadura
Original Assignee
BIOBEE TECHNOLOGIES SL
Universidad de Extremadura
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by BIOBEE TECHNOLOGIES SL, Universidad de Extremadura filed Critical BIOBEE TECHNOLOGIES SL
Publication of WO2015067834A1 publication Critical patent/WO2015067834A1/fr
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

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Classifications

    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N33/00—Investigating or analysing materials by specific methods not covered by groups G01N1/00 - G01N31/00
    • G01N33/02—Food
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
    • G01N27/02—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance
    • G01N27/026—Dielectric impedance spectroscopy

Definitions

  • the present invention relates to the field of food safety, and more specifically to a method, device and system with high portability of food and beverage quality control.
  • the concept of quality in the food industry encompasses a double dimension.
  • the first identifies the concept of quality with food safety.
  • the second is related to consumer satisfaction.
  • the responsibility for quality assurance rests primarily with the business side. This translates into the existence of a great interest on the part of said industrial segment in the search for solutions for the control of raw materials, processes and finished products, as well as for the establishment of their own mechanisms of traceability, self-control and efficiency of the show them.
  • NIRS near infrared spectroscopy
  • Bioimpedance spectroscopy is another technique that is receiving attention from the food industry, since it favors the control of manufacturing processes and the evaluation of product quality. These circumstances make it an attractive alternative to the classic control approaches of the food industry.
  • the technique is non-destructive, economical and the user does not require any previous training for its use. The tests are fast and the analytical cost is also almost non-existent, although they are invasive in the sense that in order to be carried out it is necessary to come into contact with a sample of the product.
  • bioimpedance spectroscopy has been used to analyze the physicochemical properties of materials through their correlation with the dielectric response in a given frequency range. In particular and within the food field, the technique, as described below, has been applied to the evaluation of different properties.
  • US 6,265,882 B1 describes a handheld device for measuring intramuscular fat content in meat by bioimpedance spectroscopy. It is based, like most techniques, on indirect measures, in particular and in this case on the correlation of the electrical properties of the medium, embodied in the parameters of magnitude and phase of the bioimpedance, with the intramuscular fat content.
  • the bioimpedance evaluation in the operating frequency range of the device (25 Hz-100 KHz) is performed simultaneously in two areas of the sample close to each other. This is to reduce the impact on the result of the randomness of the area of the measure if a single measure is made.
  • the device uses six puncture electrodes. Two of them for the excitation current and the other four (two pairs of sensing electrodes) for simultaneous measurement of bioimpedance in two nearby zones.
  • WO 2010/044080 A3 presents a portable device for the estimation of organoleptic parameters of the tissues of the animal in origin, as well as for the measurement of hardness (tenderness) or muscle tone.
  • the device is based on the measurement of the dielectric permittivity in a certain frequency range (0.1 Hz to 10 MHz) through the calculation of an index that reflects the electrical anisotropy of the muscle. It is carried out by measuring the module and phase of the electrical impedance in the transverse directions and parallel to the direction of the muscle fibers.
  • Muscle is a highly anisotropic medium, so that the electrical conductivity in the fiber direction is much greater than in the transverse direction. As the state of maturity progresses, the medium becomes more isotropic.
  • WO 2006/041927 A3 describes a pocket device for assessing the freshness of perishable food products.
  • the principle of operation of the device corresponds to that of an electronic nose and provides the results quickly and simply.
  • the device is provided with a sensor that reacts by varying an electrical property (resistance and / or capacity) when it is exposed to certain molecules, particles, viruses and contaminating bacteria that release food in its process towards decomposition.
  • the result provided is discrete among several possible states from maximum freshness to the state of waste.
  • US 2010/0237850 A1 presents a portable device to measure the degree of freshness of a wide variety of foods. It is based on a probe formed by two concentric metals of different nature, which form a Galvanic cell when inserted into the food and an instrument for measuring electrical potential. The comparison of the decrease in electrical potential with previously established references of this variable indirectly provides the state of freshness of the food.
  • US 7,493,798 B2 describes a technique for detecting adulteration and measuring the quality of liquids in a certain sense similar to the previous one. It basically consists of comparing the time constant associated with relaxation with a previously characterized and stored reference value. The relaxation constant associated with the fluid is determined by first generating a static charge, then injecting it into the medium and finally collecting it to perform the calculation.
  • the present invention solves the problems described above by means of a technique based on the measurement of bioimpedance spectra of both solid and liquid samples through a measuring device, said spectra being compared in processing means external to the measuring device with models Calibration stored previously.
  • a food quality measurement system which comprises a measuring device adapted to come into contact with a sample under analysis, and processing means adapted to be installed in an external and external processing device.
  • portable such as a mobile phone.
  • the measuring device in turn comprises a bioimpedance spectrometer, and optionally, a temperature sensor.
  • the measuring device comprises communication means adapted to send the measurement data (bioimpedance spectra, and where appropriate, temperature) to the processing media.
  • the processing means receive said measurements and compare them with a calibration model, previously stored in the processing device, thus determining the quality of the sample.
  • the measuring device comprises a temperature sensor
  • said temperature is used to correct deviations in the measured bioimpedance spectrum, when determining the quality of the sample.
  • a particularity of the bioimpedance spectroscopy technique is that its use for the characterization of the product composition previously requires a secondary or reference analytical method.
  • Said analytical reference method facilitates the correlation of the dielectric properties collected in the bioimpedance spectrum of the sample with its composition.
  • said dielectric properties comprise magnitude and phase angle information, using a multivariate calibration and decision-making model for analysis.
  • the processing means have access to a communications network, such as the Internet, through the portable device in which they are installed.
  • the processing means are connected through said network with an external server from which they download the calibration models associated with each type of sample to be analyzed.
  • the results of the analyzes performed by the processing means can be stored in said external server.
  • the calibration models downloaded from the external server are also used for the processing means to configure the spectrometer of the measuring device.
  • said spectrometer comprises four measuring electrodes.
  • a method of food quality control of a sample comprising the following steps: Measure bioimpedance spectra of a food sample by means of a measuring device, and in particular, by means of a bioimpedance spectrometer comprised in said measuring device.
  • the spectra comprise magnitude and phase angle information and are processed according to a multivariate calibration and decision-making model.
  • the spectra can also be measured by using four measuring electrodes together.
  • a sample temperature is measured by means of a temperature sensor comprised in the measuring device. Said temperature measurement makes it possible to compensate for deviations in the bioimpedance spectrum caused by fluctuations in the temperature of the sample.
  • Transmit the measured data (bioimpedance spectrum and temperature) to processing means, adapted to be installed in an external processing device. Said data transmission is done through a wireless connection.
  • said calibration model independent for each type of sample under analysis, is downloaded from an external server to which the processing means access through a communications network to which the processing device is connected. By means of this comparison, the food quality of the sample is determined.
  • a food quality measuring device comprising a bioimpedance spectrometer, preferably with four measuring electrodes, and communication means adapted to transmit the measured bioimpedance spectra to an external device for analysis.
  • the measuring device also comprises a temperature sensor, thus allowing compensation of the drift in the spectra produced by variations in the temperature of the sample.
  • a computer program comprising instructions executable by computer to implement the described method, when running on a computer, a digital signal processor, an application-specific integrated circuit, a microprocessor , a microcontroller or any other form of programmable hardware.
  • Said instructions may be stored in a digital data storage medium.
  • the present invention provides other important advantages such as high portability and versatility.
  • the high portability derives from the small size and weight of the measuring device, thanks to the fact that the treatment of the information and the interaction with the user (sample of results and introduction of instructions) is carried out in processing means installed in an external device.
  • the versatility results from the fact that the same device allows to operate on an open catalog of products, without downloading the appropriate calibration model or improved versions of these that are available on a mobile communications device. For all the above, together with a reduced cost, the device is useful not only for all agents in the value chain but also for consumers.
  • Figure 1 illustrates a particular implementation of the device according to an embodiment of the present invention and its application in the characterization of a sample of a liquid.
  • Figure 2 corresponds to a particular implementation of the bioimpedance spectrometer electrodes according to an embodiment of the present invention.
  • Figure 3 presents a block diagram of a particular implementation of the wireless bioimpedance spectrometer according to an embodiment of the present invention, capable of recording the temperature of the product under test.
  • Figure 4 exemplifies a Nyquist diagram (imaginary reactive part versus real resistive part of the impedance for different frequencies) corresponding to solutions with different concentrations of ethanol.
  • Figure 5 shows the flow chart of the procedure used for characterizing the composition of food products, in accordance with a particular implementation of the method according to an embodiment of the present invention.
  • Figure 1 illustrates the characterization operation of a food sample (10) with a particular embodiment of the food quality control system of the invention, which in turn follows the steps of a particular embodiment of the food quality control method of the invention.
  • Sample (10) can be both a liquid sample and a solid sample.
  • the system comprises a measuring device (20) which in turn comprises a bioimpedance spectrometer and a temperature sensor.
  • the measuring device is wirelessly communicated with processing means, installed in a processing device (30), such as a smart phone.
  • the processing means can be a computer application that can be installed on any portable programmable medium, such as electronic tablets, laptops, programmable devices designed specifically for that application, etc.
  • the spectrometer through a set of four electrodes, comes into contact with the sample (10) and generates a bioimpedance spectrum in the frequency band between 100 Hz and 3 MHz.
  • This frequency range covers the frequency band of dispersion " ⁇ ", which is one of the bands where the electrical properties -permitivity and conductivity- in the case of biological tissues change significantly in value.
  • the measurement in this frequency band is a direct evaluation of the behavior of the cell membrane, which in turn reveals useful information about the state of the sample.
  • other embodiments with a different number of electrodes are possible within the scope of the invention as claimed, as well as other embodiments with different frequency ranges for bioimpedance analysis.
  • the measured bioimpedance spectrum comprises information of magnitude and phase angle of said bioimpedance in the analysis frequency band.
  • the temperature sensor measures the temperature of the sample (10) under analysis.
  • the information captured by the measuring device (20), that is the temperature of the sample (10) and its bioimpedance spectrum, is transmitted to the processing device (30) by a wireless link governed by a communication protocol common to the two devices.
  • the configuration of the measuring device (20), and in particular of the bioimpedance spectrometer, is carried out in wirelessly from the processing device (30).
  • the communication between the measuring device (20) and the processing device (30) is carried out by means of a physical connection -a through any input such as a USB port (Universal Serial Bus) or an audio signal connector-, instead of using a wireless communications link.
  • a physical connection -a through any input such as a USB port (Universal Serial Bus) or an audio signal connector-, instead of using a wireless communications link.
  • the set of electrodes that comes into contact with the sample under characterization is considered to reside in the lower base of the measuring device (10).
  • Figure 2 corresponds to a possible embodiment of the bioimpedance spectrometer electrodes. In this particular case, it consists of four concentric electrodes in the form of rings at the bottom base, said electrodes being separated from each other by an insulating material.
  • the very low intensity electric current that is used to excite the sample (10) is applied between an external electrode (24) and an internal electrode (21), which act as excitation electrodes.
  • the frequency of this electrical excitation current varies sequentially in a certain range.
  • Two intermediate concentric electrodes (23) and (22) act as sensing electrodes, picking up the potential whose difference is intended to be measured.
  • the four electrodes are electrically connected, through the interior of the rod, to the bioimpedance spectrometer circuitry, which resides at the opposite end to the concentric electrodes in the measuring device (20).
  • Note that other different architectures for the electrodes can be adopted within the scope of the invention as claimed. It is also possible to opt for interchangeable electrode architectures depending on the type of product, without altering the concept of the proposed system operation.
  • Figure 2 further shows a temperature sensor (25), in this particular case located inside the concentric electrodes of the measuring device (20).
  • the measurement of the temperature through said temperature sensor (25) subsequently makes it possible to compensate in the processing device (30) the deviations that said temperature can induce in the bioimpedance spectra, and therefore, in the characterization of the composition of the sample (10).
  • the measuring device (20) is responsible for obtaining the bioimpedance parameters of the food sample (10) -magnitude and phase angle for different frequencies of the excitation current in the operating band-, in addition to the temperature of the same, and transmit them to the processing device
  • FIG. 3 shows the block diagram of the measuring device (20) capable of measuring bioimpedance spectra and sample temperature.
  • the processing device (30) comprises a first block (26), which in turn comprises a specific application integrated circuit together with an excitation current generator circuit programmable in magnitude and frequency.
  • the measuring device comprises a microcontroller (27), radio frequency means (29) with transmission and reception capabilities, and a signal conditioning circuit (28) connected to the temperature sensor (25).
  • a microcontroller 27
  • radio frequency means with transmission and reception capabilities
  • a signal conditioning circuit connected to the temperature sensor (25).
  • other means of transmitting and receiving data can be used, such as a bluetooth connection or any other alternative communication system, it being preferable that said communication be wireless to facilitate the use and portability of the system.
  • the excitation current generating circuit is controlled by the microcontroller (27).
  • the excitation current of sinusoidal character, is applied to the food sample (10) through the excitation electrodes (21, 24).
  • the resulting voltage is collected through the sensing electrodes (22, 23).
  • the difference between the voltages measured by the sensing electrodes is processed in an analog input section implemented in the specific application integrated circuit.
  • the analog input section provides as outputs two voltages of continuous (DC), proportional to the magnitude and phase angle, respectively, of the bioimpedance of the biological sample (10).
  • the measuring device (20) is provided with a temperature sensor (25) (for example, a thermistor) and a signal conditioning section (28).
  • the output voltage of the circuit (28) is transmitted to the microcontroller (27) for conversion to a digital code and for subsequent transmission, together with the bioimpedance spectrum, to the device processed (30) through the radiofrequency section (29).
  • the microcontroller (27) controls the excitation current source that is applied to the sample according to a configuration stored in a calibration model that is transmitted from the mobile communications unit (30).
  • Said calibration model comprises frequency and current intensity information for each analysis that makes up the spectrum, and is dependent on the type of sample (10) under analysis.
  • the microcontroller (27) converts the voltages corresponding to the magnitude and phase angle of the bioimpedance to each of the bioimpedance analyzes that make up the spectrum into a digital code.
  • the radio frequency section (29) receives from the processing device (30) the configuration parameters of the spectrometer for the adequate generation of the bioimpedance spectrum corresponding to the type of food sample under test.
  • the radiofrequency section (29) transmits to the processing device (30), together with the sample temperature, the measurements obtained from bioimpedance that make up the spectrum.
  • the processing device (30) performs a double function. First, prior to performing bioimpedance measurements of the measuring device (20), configure the spectrometer according to the corresponding calibration model. Secondly, once the bioimpedance spectrum and temperature have been received, the processing device (30) is responsible for processing and interpreting the measurements, displaying the results of the characterization on a screen and, optionally, storing said results on its own measuring device (30) and / or transmit them to a remote server.
  • Figure 4 shows the Nyquist diagram - imaginary reactive part ⁇ ( ⁇ ) versus real resistive part R (Q) of the impedance for different frequencies - corresponding to ethanol solutions with different concentration values (C) .
  • the diameter of each semicircle decreases as the value (C) of the alcohol concentration does the same.
  • the development of the calibration / prediction model for each type of product requires a reference analysis with a secondary analytical method.
  • the general purpose of a calibration model is to correlate certain properties thereof - in this case electrical properties that are reflected in the bioimpedance spectrum - with the physicochemical properties or parameters of interest.
  • the models are statistical models based on multivariate techniques. Once the statistical model has been generated, it is subsequently used in the prediction of the properties of new samples from its bioimpedance spectrum. The development of multivariate models requires the participation of qualified technical personnel.
  • the calibration models used in the present invention can be generated using different techniques that are widely known and used in the state of the art (for example, in near infrared spectrometry).
  • the processing unit (30) has a memory in which the calibration model corresponding to the type of product to be characterized is stored, prior to the application of the system on the sample (10).
  • the calibration model can be downloaded, for example, from an external server through communication networks, such as the internet.
  • the Internet connectivity of the processing device (30) provides the measuring device (20) with high versatility, derived from the possibility of downloading calibration models of other food products or new improved versions of existing models.
  • the calibration models in addition to providing a reference to compare the bioimpedance spectra measured by the spectrometer, provide specific spectrometer configuration parameters for each type of product, such as frequencies and intensities of the excitation current for the analyzes .
  • Figure 5 shows the flow chart of the process used by the system of the invention for characterizing the composition of food products.
  • the procedure comprises the following steps: a) Discharge (40) of the calibration model into the processing device (30) corresponding to the type of food sample (10) to be characterized. This step is only necessary if the calibration model is not previously stored in the processing device (30). b) Remote configuration (41) of the bioimpedance spectrometer. For this, the calibration model is executed on the processing means installed in the processing device (30) and the specific parameters of the bioimpedance spectrometer configuration are transmitted via the wireless protocol. Such configuration parameters are typically those values corresponding to the frequencies of the electrical excitation current and the intensity thereof for each bioimpedance analysis that makes up the spectrum of the sample type.

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  • Chemical & Material Sciences (AREA)
  • Physics & Mathematics (AREA)
  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Biochemistry (AREA)
  • Food Science & Technology (AREA)
  • Analytical Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • General Health & Medical Sciences (AREA)
  • General Physics & Mathematics (AREA)
  • Immunology (AREA)
  • Pathology (AREA)
  • Medicinal Chemistry (AREA)
  • Spectroscopy & Molecular Physics (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • Investigating Or Analysing Materials By Optical Means (AREA)

Abstract

La présente invention concerne un procédé, un dispositif et un système d'analyse de la qualité des aliments reposant sur la mesure de spectres de bioimpédance d'un échantillon (10) et sur la comparaison desdits spectres à un modèle d'étalonnage de référence. La mesure du spectre est effectuée au moyen d'un dispositif de mesure (20), relié sans fil à des moyens de traitement chargés d'effectuer la comparaison. Les moyens de traitement peuvent être installés dans un dispositif portatif pouvant communiquer avec un serveur externe à partir duquel peuvent être téléchargés et actualisés les modèles d'étalonnage propres à chaque type d'échantillon.
PCT/ES2014/070825 2013-11-05 2014-11-05 Procédé, dispositif et système de contrôle de la qualité des aliments Ceased WO2015067834A1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
ES201301058A ES2535280B1 (es) 2013-11-05 2013-11-05 Método, dispositivo y sistema de control de calidad alimentaria
ESP201301058 2013-11-05

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WO2015067834A1 true WO2015067834A1 (fr) 2015-05-14

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105241826A (zh) * 2015-10-13 2016-01-13 惠州Tcl移动通信有限公司 智能移动终端及其进行食品检测的方法

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2009059351A1 (fr) * 2007-11-05 2009-05-14 Impedimed Limited Détermination de l'impédance
ES2401286A2 (es) * 2011-08-30 2013-04-18 Universidad De Extremadura Unidad, sistema modular y procedimiento para la medición, procesamiento y monitorización remota de bioimpedancia eléctrica

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2009059351A1 (fr) * 2007-11-05 2009-05-14 Impedimed Limited Détermination de l'impédance
ES2401286A2 (es) * 2011-08-30 2013-04-18 Universidad De Extremadura Unidad, sistema modular y procedimiento para la medición, procesamiento y monitorización remota de bioimpedancia eléctrica

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
MASOT: "Desarrollo de un sistema de medida basado en espectroscopia de impedancia para la determinación de parámetros fisicoquimícos en alimentos''.", TESIS., 20 July 2010 (2010-07-20), Retrieved from the Internet <URL:httos://www.educacion.es/teseo/mostrarRef.d0?ref=888348> [retrieved on 20141222] *

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105241826A (zh) * 2015-10-13 2016-01-13 惠州Tcl移动通信有限公司 智能移动终端及其进行食品检测的方法

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Publication number Publication date
ES2535280B1 (es) 2016-03-15
ES2535280A2 (es) 2015-05-07
ES2535280R2 (es) 2015-05-27

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