CN103412030A - Grease detection method based on volt-ampere type electronic tongue - Google Patents
Grease detection method based on volt-ampere type electronic tongue Download PDFInfo
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Abstract
The invention relates to a grease detection method based on a volt-ampere type electronic tongue, and the method is particularly applicable to detection on edible vegetable oil. The detection method is further applicable to property identification and detection on other liquid samples. The invention discloses a volt-ampere type electronic tongue grease detection method based on adjustable cyclic volt-ampere scanning potential, aiming at the high viscosity and the low conductivity of the oil, and being designed for solving the problem that the great difficulty is caused when a volt-ampere type electronic tongue system is directly put into grease for detection. The method comprises a multi-sensor array, a hardware circuit and intelligent detection software, wherein the multi-sensor array is in a three-electrode system structure consisting of a working electrode, an auxiliary electrode and a reference electrode, and is put into a solution to be detected; a signal acquisition system mainly comprises a temperature control circuit, a motivation signal generation circuit, a signal conditioning circuit and a data acquisition circuit; the intelligent detection software mainly comprises sensor array optimization, motivation signal parameter setup, data acquisition software and mode recognition algorithms. The method is capable of effectively carrying out specificity difference identification on the grease, and has the characteristics that the multi-sensor array is flexibly selected, the motivation signals are intelligently adjusted, the detection is convenient and rapid, and the like.
Description
Technical field
The present invention relates to a kind of detection methods of lipid based on volt-ampere electronic tongue, especially be applied to edible vegetable oil and detect.Detection method of the present invention can also be for other fluid sample overall permanence identification, so for qualitative, quantitatively reach quality control.
Background technology
Electronic tongues is that a kind of low selectivity, many sensor arrays non-specific, mutual sensitivity utilized are basis, the global feature response signal of the unknown fluid sample of sensing, the methods such as Applied Chemometrics, sample is carried out to the detection technique of pattern-recognition and qualitative and quantitative analysis, electronic tongues mainly is comprised of taste sensor array, signal acquiring system and pattern recognition system three parts.Taste sensor array is the core component of electronic tongues system, and the more taste sensor array of research is mainly electric potential type, volt-ampere type and impedance spectral pattern both at home and abroad at present.The working electrode that volt-ampere type sensor often uses is bare metal electrode or modified electrode etc.The added step electromotive force of volt-ampere type sensor mainly contains cyclic voltammetric, routine significantly pulse and multifrequency pulse voltammetry etc.
In most of electronic tongues application systems, the sample solution of detection is aqueous medium, and as fruit juice, tealeaves, wine or other alcoholic beverage, when the electronic tongues system detected these sample solutions, solution can provide fully good electric conductivity.But for high viscosity as grease, low electric conductivity and impotentia, dissolve the detection sample of the standard electrolyte of sufficient amount, the application difficulty of electronic tongues detection technique increases greatly.
P é ter M é sz á ros research group of Budapest Kao Wenniusi university adopts French Alpha Astree electronic tongues system to distinguish and specificity analysis to corn oil, sunflower oil, olive oil and palm oil and by the different proportion miscella.The taste sensor array of France Alpha Astree electronic tongues system is electric potential type, and the electric potential signal of pick-up transducers is as detection signal.This electronic tongues system is in grease detects, and the oil sample pre-treating method is mainly the ethanol extraction method, the shortcoming such as have unavoidably that the pre-treatment time is long, the sample consumption is large, not easy cleaning and maintenance of sensor, serviceable life are short.
The Paolo Oliveri research group of Italy Genoa university has designed a kind ofly take golden microelectrode and is two electrode electronic tongues system direct-detection vegetable oil samples of working electrode, successfully distinguishes corn oil and the virgin oil of different geographic origin, different qualities.This electronic tongues system adopts cyclic voltammetry as detection signal.Voltammetry has solved the shortcoming of electric potential type sensor oil sample complex pretreatment, but this electronic tongues system sensor is single, pumping signal is single, can't carry out the corresponding adjusting of pumping signal according to different oil sample response characteristics and carry out characteristic optimizing analysis, Intelligent Measurement.
At present the electronic tongues system applies also having been adopted to decorating carbon paste electrode in oil quality detects is working electrode, still has the defects such as the sensor preparation is complicated, serviceable life is short.
Summary of the invention
In order to address the above problem, the preferred embodiments of the invention provide a kind of detection methods of lipid based on volt-ampere electronic tongue, especially are applied to edible vegetable oil and detect.The combination cyclic voltammetry scan electromotive force of take is pumping signal, response current signal in Real-time Collection solution system to be measured produces under the pumping signal effect electrochemical reaction process, adopt the pattern-recognition scheduling algorithm to carry out qualitative or quantitative test to property difference and content of material between the global feature of solution to be measured, material.
A kind of based on the volt-ampere electronic tongue detection methods of lipid, for oily high viscosity and low electric conductivity, the volt-ampere electronic tongue system directly is placed in to the grease detection and has great difficulty and invent.Comprise: multisensor array, signal acquiring system and Intelligent Measurement software.Wherein, multisensor array forms the three-electrode system structure by working electrode, auxiliary electrode and contrast electrode, is placed in solution to be measured; Signal acquiring system comprises that mainly pumping signal produces circuit, signal conditioning circuit and data acquisition circuit; Intelligent Measurement software mainly comprises sensor array optimization, the setting of pumping signal parameter, data acquisition software, algorithm for pattern recognition.
Described volt-ampere electronic tongue system ultimate principle is the thought by the galvanochemistry voltammetry, multisensor array is placed in to solution to be measured, on working electrode, add the cyclic voltammetry scan electromotive force, the difference that produces the size of current of redox reactions by detecting different solution to be measured is carried out the characteristic of qualitative and quantitative analysis sample.
Described combination cyclic voltammetry scan electromotive force is as pumping signal, and scanning voltage basic waveform is isosceles triangle, and a test period interscan voltage range is-2-2V, sweep speed variation range 50mV/s-500mV/s.
The multisensor array that described volt-ampere electronic tongue system adopts is three-electrode structure: working electrode, contrast electrode and auxiliary electrode.
Described working electrode is the one or more combination of platinum, gold, silver, palladium, titanium, tungsten disc electrode, while or time-sharing work.
Described contrast electrode is the Ag/AgCl electrode.
Described auxiliary electrode is platinum post electrode.
Described signal acquiring system comprises that mainly pumping signal produces circuit, signal conditioning circuit and data acquisition circuit.Pumping signal produces circuit and is responsible for producing the required combination cyclic voltammetry scan electromotive force of solution to be measured; Due to the virtual instrument data collecting card, can not directly gather the current signal of solution electronic tongues response to be measured, so in circuit, increased signal conditioning circuit, making the signal gathered is voltage signal, and signal conditioning circuit comprises potentiostatic circuit, current-to-voltage converting circuit, signal amplification circuit, signal filter circuit; Data acquisition circuit is responsible for gathering the voltage signal of solution electronic tongues response to be measured.
Described Intelligent Measurement software comprises that mainly sensor array optimization module, pumping signal parameter arrange module, data acquisition module, pattern recognition module.For testing sample solution, not all sensor all can produce effectively stable electronic tongues response, can to sensor array, adjust by experiment, the sensor array optimization module is for selecting the 6 road analog input channels that are connected with working electrode, can single working electrode work, but also the multiplex (MUX) makes electrode simultaneously or time-sharing work; The pumping signal parameter arranges the data that module collects by the analytic signal acquisition system, and cyclic voltammetry scan electromotive force parameter is adjusted and arranged; Data acquisition module is for from working electrode, gathering the response current signal produced by solution oxide reduction reaction to be measured, but multichannel gathers simultaneously; Pattern recognition module comprises that feature extraction and pattern-recognition realize, application mode identification or chemometrics method carry out analyzing and processing to the characteristic value data extracted, and set up the qualitative/quantitative analytical model, thereby realize solution Quality Detection to be measured or quantitative test.
The present invention has following feature and advantage:
A. taste sensor array is the bare metal electrode, electrode clean, the preparation simple and convenient;
B. taste sensor array can be selected flexibly according to actual detection material system, can single/multi-electrode work, and can be simultaneously or time-sharing work;
C. the different characteristics for solution to be measured changes pumping signal, and pumping signal is combination cyclic voltammetry scan electromotive force, and wherein, the parameters such as scanning voltage, sweep speed, cycle index are adjustable, to obtain solution maximum fault information to be measured;
D. all data of signal acquiring system collection are directly called in Intelligent Measurement software, do not need to consider application secondary software and data-interface reunification;
E. have analysis speed fast, highly sensitive, obtain the characteristics such as solution to be measured contains much information, be applicable to the analysis of on-the-spot oil quality detection and identification, especially be applied to edible vegetable oil and detect.
Detailed description from below with reference to accompanying drawing and preferred embodiment, will be expressly understood other characteristics of the present invention, key element and characteristic and advantage more.
The accompanying drawing explanation
Fig. 1 is structural representation of the present invention.
Fig. 2 is the volt-ampere response curves of six kinds of working metal electrodes in soybean oil.
Fig. 3 is single electrode work combination cyclic voltammetry scan potential waveform.
Fig. 4 is multi-electrode work combination cyclic voltammetry scan potential waveform.
Fig. 5 is based on different edible vegetable oil under Fig. 3 pumping signal and distinguishes identification result figure.
Fig. 6 is based on different edible vegetable oil under Fig. 4 pumping signal and distinguishes identification result figure.
Embodiment
Basic thought of the present invention: by the redox reaction current signal of a kind of volt-ampere electronic tongue system acquisition generation under the excitation of combination cyclic voltammetry scan electromotive force; Described current signal is carried out to the eigenwert extraction; Application mode identification or chemometrics method carry out analyzing and processing to the characteristic value data extracted, thereby realize solution Quality Detection to be measured or quantitative test.
Wherein, described solution to be measured is the mixed solution of the different types of edible vegetable oil of 40ml and 1.3g ionic liquid at room temperature, the three hexyl phosphine tetradecylic acids in the last of the ten Heavenly stems that ionic liquid at room temperature adopts U.S. strem company to produce, directly with edible vegetable oil, mix, through ultrasonic processing 5min homogenize, standing 15min before voltammertry.
Fig. 1 is structural representation of the present invention.Comprise: multisensor array, signal acquiring system and Intelligent Measurement software.Wherein, multisensor array forms the three-electrode system structure by working electrode, auxiliary electrode and contrast electrode, is placed in solution to be measured; Signal acquiring system comprises that mainly pumping signal produces circuit, signal conditioning circuit and data acquisition circuit; Intelligent Measurement software mainly comprises sensor array optimization, the setting of pumping signal parameter, data acquisition software, algorithm for pattern recognition.
Multisensor array forms the three-electrode system structure by working electrode, auxiliary electrode and contrast electrode, and working electrode is
The one or more combination of 2mm platinum, gold, silver, palladium, titanium, tungsten disc electrode, contrast electrode is
6mm Ag/AgCl electrode, auxiliary electrode are 1
5mm platinum post electrode.Each working electrode even circumferential distributes, and auxiliary electrode and each working electrode are equidistant.Electrode clean adopts ethanol solution.
As shown in Figure 1, signal acquiring system comprises that mainly pumping signal produces circuit, signal conditioning circuit and data acquisition circuit.Pumping signal produces circuit and is responsible for producing the required combination cyclic voltammetry scan electromotive force of solution to be measured; Due to the virtual instrument data collecting card, can not directly gather the current signal of solution electronic tongues response to be measured, so in circuit, increased signal conditioning circuit, making the signal gathered is voltage signal, and signal conditioning circuit comprises potentiostatic circuit, current-to-voltage converting circuit, signal amplification circuit, signal filter circuit; Data acquisition circuit is responsible for gathering the voltage signal of solution electronic tongues response to be measured.
Described combination cyclic voltammetry scan electromotive force is as pumping signal, and scanning voltage basic waveform is isosceles triangle, and a test period interscan voltage range is-2-2V, sweep speed variation range 50mV/s-500mV/s.The generation form of pumping signal has following two kinds:
A. by virtual instrument data collecting card+LabVIEW software programming, realize;
B. by hardware circuits such as function signal circuit for generating, FM circuit and modulation circuits, form.
Fig. 1 is in the present embodiment, adopts virtual instrument data collecting card+LabVIEW software programming to complete the generation of pumping signal.In signal acquiring system, data acquisition circuit is realized based on the Virtual Instrument LabVIEW platform, and data collecting card adopts the USB6251 of America NI company.Signal conditioning circuit is realized by drawing together the hardware circuits such as potentiostatic circuit, current-to-voltage converting circuit, signal amplification circuit, signal filter circuit.
Described Intelligent Measurement software is write based on LabVIEW8.6, comprises that mainly sensor array optimization module, pumping signal parameter arrange module, data acquisition module, pattern recognition module.The sensor array mode of operation has following three kinds:
A. combine the lower single electrode work of electromotive force excitation;
B. combining electromotive force excitation lower sensor array works simultaneously;
C. various combination electromotive force excitation lower sensor array time-sharing work.
To be platinum, silver, gold, palladium, titanium and six kinds of working electrodes of tungsten be-2-2V at scanning voltage to Fig. 2, and sweep speed is to the volt-ampere response curve of certain soybean oil under the cyclic voltammetry scan electromotive force excitation of 100mV/s.After in edible oil sample, adding ionic liquid at room temperature, show good electrochemical response window, necessary condition is provided in the detection of edible oil sample for volt-ampere electronic tongue.
Fig. 3 is in the present embodiment, adopt the lower single electrode mode of operation of combination electromotive force excitation, wherein, the optional one of platinum, silver, gold, palladium, titanium and six kinds of working electrodes of tungsten within a test period, scanning voltage scope-2-2V is optional, and sweep speed 50mV/s-500mV/s is optional.
Fig. 4 is in the present embodiment, the work of various combination electromotive force excitation lower sensor array time-sharing.Wherein, but within a test period six kinds of working electrode time-sharing works, different test duration sections can have the different operating electrode to work under the excitation of various combination electromotive force, scanning voltage scope-2-2V is optional, sweep speed 50mV/s-500mV/s is optional.Signal acquiring system gathers the response signal of all the sensors array, then based on the Whole Response signal, carries out pattern-recognition or other qualitative and quantitative analysis.
Use detection methods of lipid of the present invention to detect and analyze different edible vegetable oil (as shown in the table):
Choose all food plant oil samples in table and detect and analyze, different types of edible vegetable oil and ionic liquid at room temperature are mixed into to solution to be measured, the sensor array mode of operation adopts shown in Figure 3.Wherein, working electrode is platinum electrode, 50mV/s, and tri-kinds of cyclic voltammetry scan electromotive force combinations of 100mV/s and 200mV/s are as pumping signal, and every kind of sweep speed circulates twice.Scanning voltage scope-2-2V.Signal acquiring system gathers the response signal of platinum electrode under the excitation of combination electromotive force, obtains the sample data matrix.Then Intelligent Measurement software extracts eigenwert based on these data, and 12 kinds of different edible vegetable oils are carried out to the PCA analysis, and Fig. 5 is based on the lower 12 kinds of edible vegetable oils of Fig. 3 pumping signal and distinguishes identification result figure.In figure, each sample repeats to measure 5 times, and each circle represents the interior difference of the sample of same sample, between circle, represents the whole difference between different samples.The result demonstration, different samples have different distributed areas, use detection methods of lipid of the present invention to distinguish the edible oil of the different material place of production, different cultivars, and it is remarkable to distinguish effect.
Due to the same solution susceptibility difference to be measured of different operating electrode pair, the size of response signal is also different, so that single working electrode can obtain the sample Global Information is limited, and under proper testing, as while single working electrode job insecurity occurring, very large change will occur in Measurement results.In the present embodiment, choose all food plant oil samples in table and detect and analyze, different types of edible vegetable oil and ionic liquid at room temperature are mixed into to solution to be measured, the sensor array mode of operation adopts shown in Figure 4.Wherein, working electrode is platinum electrode Pt, silver electrode Ag, gold electrode Au after optimizing, it is 100mV/s and the excitation of 200mV/s combination electromotive force that platinum electrode is operated in sweep speed, it is the excitation of 500mV/s combination electromotive force that silver electrode Ag is operated in sweep speed, it is the excitation of 100mV/s combination electromotive force that gold electrode Au is operated in sweep speed, time-sharing work, every kind of sweep speed circulation primary.Scanning voltage scope-2-2V.
Signal acquiring system gathers the response signal of compound electrode under the excitation of combination electromotive force, obtains the sample data matrix.Then Intelligent Measurement software extracts eigenwert based on these data, and 12 kinds of different edible vegetable oils are carried out to the PCA analysis, and Fig. 6 is based on the lower 12 kinds of edible vegetable oils of Fig. 4 pumping signal and distinguishes identification result figure.In figure, each sample repeats to measure 5 times, and each circle represents the interior difference of the sample of same sample, between circle, represents the whole difference between different samples.The result demonstration, the sample room difference of same sample diminishes, and different samples have different distributed areas, use detection methods of lipid of the present invention to distinguish the edible oil of the different material place of production, different cultivars, and it is remarkable to distinguish effect.
The invention is not restricted to above-mentioned each preferred embodiment, can in scope of the present invention, make various remodeling.
By above, to specific descriptions of the present invention, show the feature different from other volt-ampere electronic tongue and advantage.Although more than described the preferred embodiments of the invention, be appreciated that those skilled in the art can make various remodeling and variation under the prerequisite do not departed from the scope of the present invention.Therefore, scope of the present invention is limited by following claim.
List of references
[1]?Paolo?Oliveri,?M.Antonietta?Baldo,Salvatore?Daniele?,?et?al.?Development?of?a?voltammetric?electronic?tongue?for?discrimination?of?edible?oils?[J].?Anal?Bioanal?Chem,2009,395:1135-1143.
[2]?Péter?Mészáros.Analysis?of?Edible?Oil?Quality?Characteristics?Tested?on?Electronic?Tongue?System.?ASAE?Annual?International?Meeting，2005,?1-8.
[3]?Apetrei,C.,?Rodriguez-Mendez,?M.L.,?De?Saja,?J.A.?Modified?carbon?paste?electrodes?for?discrimination?of?vegetable?oils?[J].?Sensors?and?Actuators?B-Chemical,?2005,?111:403-409.
[4]?Apetrei,?C.,?Gutierez,?F.,?Rodr'iguez-M'endez,?et?al.?Novel?method?based?on?carbon?paste?electrodes?for?theevaluation?of?bitterness?in?extra?virgin?olive?oils?[J].?Sensors?and?Actuators?B,2007,121(2):?567-575.
[5]?Rodriguez-Mendez,?M.L.,.Apetrei,?C.,?et?al.?Evaluation?of?the?polyphenolic?content?of?extra?virgin?olive?oils?using?an?array?of?voltammetric?sensors?[J].?Electrochimica?Acta,?2008(53):?5867-5872.
[6] Tian Shiyi. multifrequency pulse electronic tongue system constructing and application [D]. Zhejiang Prov Industrial And Commercial University, 2007.
[7] Wei Zhenbo. the research and development of volt-ampere electronic tongue and the application in food inspection [D] thereof. Zhejiang University, 2011
Claims (9)
1. detection methods of lipid based on volt-ampere electronic tongue, this feature comprises:
Multisensor array, signal acquiring system and Intelligent Measurement software, wherein, multisensor array forms the three-electrode system structure by working electrode, auxiliary electrode and contrast electrode, is placed in solution to be measured; Signal acquiring system comprises that mainly temperature-control circuit, pumping signal produce circuit, signal conditioning circuit and data acquisition circuit; Intelligent Measurement software mainly comprises sensor array optimization, the setting of pumping signal parameter, data acquisition software, algorithm for pattern recognition.
2. volt-ampere electronic tongue as claimed in claim 1 is characterized in that:
Described working electrode is that the one or more combination of platinum, gold, silver, palladium, titanium, tungsten disc electrode becomes multisensor array, while or time-sharing work.
3. volt-ampere electronic tongue as claimed in claim 1, preferably, described auxiliary electrode is platinum post electrode.
4. volt-ampere electronic tongue as claimed in claim 1, preferably, described contrast electrode is the Ag/AgCl electrode.
5. solution to be measured as claimed in claim 1, it is characterized in that: solution is the mixed solution of different types of oil sample to be measured and ionic liquid at room temperature, ionic liquid at room temperature in solution as supporting electrolyte, it shows good dissolving power to inorganic and organic material, non-volatile, toxicity is little, good conductivity, have wider electrochemical window, can directly with oily, mix, can select three hexyl phosphine tetradecylic acids in the last of the ten Heavenly stems or other suitable ionic liquid as supporting electrolyte to improve oily electric conductivity.
6. pumping signal generation circuit as claimed in claim 1 and data acquisition circuit are based on virtual instrument platform and are not limited to this a kind of hardware platform.
7. pumping signal as claimed in claim 1 is the scanning electromotive force of Linear Circulation voltammetry, definite instructions that is not limited only to of scanning voltage waveform is described scope, wherein, scanning voltage is adjustable, sweep speed is adjustable, excitation signal parameter (scanning voltage is adjustable, sweep speed etc.) all can arbitrarily regulate, combines or do not regulate according to the reality test.
8. algorithm for pattern recognition as claimed in claim 1 is not limited only to instructions and describes scope, also can adopt least square method, support vector machine etc. solution to be measured to be carried out to the index of quality quantitative test such as peroxide value, acid value, carry out the analyses such as grease blending, adulterated, waste oil or quality control.
9. the detection methods of lipid based on volt-ampere electronic tongue of the present invention has comprised the detection methods of lipid based on the galvanochemistry voltammetry, be about to multisensor array and be placed in solution to be measured, on working electrode, add the combination cyclic voltammetry scan electromotive force described in claim 7, detect the size of current that different solution to be measured produces redox reaction.
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| CN104076069A (en) * | 2013-12-04 | 2014-10-01 | 浙江工商大学 | Pork storage time detection method |
| CN110070069A (en) * | 2019-04-30 | 2019-07-30 | 重庆大学 | A kind of Classification of Tea method based on convolutional neural networks Automatic Feature Extraction |
| CN110954584A (en) * | 2019-11-15 | 2020-04-03 | 浙江省农业科学院 | Taste testing method and verification method based on electronic tongue |
| CN111896679A (en) * | 2020-07-01 | 2020-11-06 | 广东轻工职业技术学院 | Method for rapidly identifying processing mode of camellia seed oil and predicting acid value and peroxide value based on taste fingerprint spectrum |
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| GR20210100167A (en) * | 2021-03-17 | 2022-10-10 | Εθνικο Και Καποδιστριακο Πανεπιστημιο Αθηνων, | Electrochemical system and method for the detection of adulteration of extra virgin olive oil |
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| CN111896679A (en) * | 2020-07-01 | 2020-11-06 | 广东轻工职业技术学院 | Method for rapidly identifying processing mode of camellia seed oil and predicting acid value and peroxide value based on taste fingerprint spectrum |
| CN112710533A (en) * | 2021-01-19 | 2021-04-27 | 浙江大学 | Bionic taste sense system for food detection |
| GR20210100167A (en) * | 2021-03-17 | 2022-10-10 | Εθνικο Και Καποδιστριακο Πανεπιστημιο Αθηνων, | Electrochemical system and method for the detection of adulteration of extra virgin olive oil |
| GR1010451B (en) * | 2021-03-17 | 2023-05-03 | Εθνικο Και Καποδιστριακο Πανεπιστημιο Αθηνων, | Electrochemical system and method for the detection of adulteration of extra virgin olive oil |
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Application publication date: 20131127 |