CN104880419A - Photoacoustic combined spectroscopy food and medicine ingredient content fast detection device and method - Google Patents
Photoacoustic combined spectroscopy food and medicine ingredient content fast detection device and method Download PDFInfo
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Abstract
The invention discloses a photoacoustic combined spectroscopy food and medicine ingredient content fast detection device and method. The device comprises a light source radiation unit, a detection room unit, a spectroscopy light splitting unit, a light source detection unit, a signal processing unit, a signal control unit and a signal display unit. The device and the method have the following beneficial effects that on one hand, the characteristics of convenience and high speed when feature wavelength is found by spectroscopy, the time is greatly saved, and great convenience is brought to the feature wavelength selection in a photoacoustic detection method, so that the detection efficiency is greatly improved; on the other hand, the photoacoustic technology is used for carrying out qualitative and quantitative detection on detected substances, and the inference due to various groups of scattered light in detected substances in spectroscopy is avoided, so that the detection accuracy is greatly improved.
Description
Technical field
The present invention relates to food and medicine quality testing field, be specially a kind of food and medicine component and content device for fast detecting of optoacoustic coupling spectroscopic methodology.
Background technology
Raising along with people's living standard and the attention to health, food and drug quality problems become the focus of social concerns day by day.Recent related food and drug quality problems have exposure repeatly; such as: " cadmium rice " event, " malicious milk powder " event, " melamine " event, " toxic capsule " event etc.; similar event has had a strong impact on social stability, causes the trust crisis of people to associated production producer and superintendent office.
Food and drug safety are matters vital to national well-being and the people's livelihood, and the detection method that current quarantine departments often adopts is mainly by vision subjective judgement, chemical-agent technique and instrument detection method.Because vision subjective judgement is subject to the impact of experience level and the subjective meaning, metrical error is relatively large; Chemical-agent technique, due to the incomprehensiveness to tested composition, makes the testing process of this method very long, consumes more human and material resources and financial resources, and due to the interference of chemical reagent composition, bring impact can to the accuracy detected; For instrument detection method, at present conventional detecting instrument is the instrument such as efficient liquid phase, gas chromatograph or mass spectrometry mainly, because such instrumentation is complicated, need loaded down with trivial details pre-treatment, and need professional just can carry out detection operation, and price is relatively costly, make the utilization rate of this quasi-instrument and popularization not high.
Recently, nondestructiving detecting means is more and more favored, and its reason is that the method has the features such as harmless, quick, portable and workable, and wherein representative have optical non-destructive detection method, as; Ultraviolet spectroscopy, infra-red sepectrometry, Raman spectroscopy etc.Although spectroscopic methodology has green, fast and the feature such as harmless, but due to measured matter component diversity, the interference of polycomponent spectrum can be caused, simultaneously because spectroscopic methodology is in the intrinsic spectra overlapping effect of characteristic spectral range, the precision and stability of spectrum detection method is affected.And optoacoustic Dynamic Non-Destruction Measurement is different from spectral method of detection, this technology utilizes photic ultrasonic technique, that is: pulsed laser radiation measured matter is utilized, thermal expansion is fast produced owing to making measured matter local to the absorption of characteristic wavelength laser energy, thus produce ultrasonic mechanical wave, by catching photic ultrasound wave and utilizing signal analysis technology just can be finally inversed by the information such as composition and content of measured matter.Be ultrasonic signal due to what obtain, so the scattered light interference that spectroscopic methodology brings greatly can be overcome, make to detect stability and accuracy is improved.But when utilizing photoacoustic technique to detect, its component and content cannot be judged by real-time optoacoustic time-domain signal, and need to be analyzed by the optoacoustic value obtained under some characteristic wavelength.But due in advance and do not know the characteristic wavelength of tested component, so need to gather the photoacoustic signal of each wavelength, then therefrom characteristic wavelength is found out, make testing process consuming time longer, and the correctness that characteristic wavelength is selected directly affects reliability and the accuracy of the detection of tested component.Therefore, need to seek a kind ofly to improve the efficiency of optoacoustic Non-Destructive Testing and the method for accuracy.
Summary of the invention
The invention provides one both improved detection efficiency to overcome above-mentioned deficiency, ensure again food and medicine component and the content device for fast detecting of the optoacoustic coupling spectroscopic methodology of testing result accuracy.
For solving the problems of the technologies described above, realize above-mentioned purpose, the present invention is achieved through the following technical solutions:
A kind of food and medicine component of optoacoustic coupling spectroscopic methodology and content device for fast detecting, comprise radiation of light source unit, sensing chamber's unit and signal display unit, also comprise spectrum unit, optoacoustic detection unit, signal processing unit and signaling control unit, described radiation of light source unit, sensing chamber's unit and spectrum unit set gradually along optical propagation direction, the photoacoustic signal output terminal of described sensing chamber unit is connected with the photoacoustic signal input end of optoacoustic detection unit, the electrical signal of described spectrophotometric unit and optoacoustic detection unit is all connected with the electric signal input end of signal processing unit, the signal input part of described signaling control unit is connected with the signal output part of signal processing unit, the control signal input end of described signal display unit and radiation of light source unit is all connected with the control signal output terminal of signaling control unit.
The present invention has following beneficial effect:
Owing to adopting optoacoustic method and spectroscopic methodology coupling technique, this pick-up unit and detection method are had concurrently the advantage of photo-acoustic detection and spectral detection, on the one hand, spectroscopic methodology is utilized to find characteristic wavelength feature easily and fast, greatly save and facilitate the selection of characteristic wavelength in optoacoustic detection method, detection efficiency is improved greatly; On the other hand, utilize photoacoustic technique to carry out quantitative and qualitative analysis detection to measured matter, avoid the interference that in spectroscopic methodology, in measured matter, polycomponent scattered light brings, accuracy in detection is improved greatly.Compared with classic method, the method has that harmless, quick, operability is stronger, accuracy more high, and this also makes this device and detection method have better practicality and applicability.
Accompanying drawing explanation
Fig. 1 is principle schematic of the present invention.
Fig. 2 is flat reflective grating beam splitting schematic diagram.
Fig. 3 is concave reflective grating beam splitting schematic diagram.
Fig. 4 is volume holographic transmission-type grating light splitting schematic diagram.
Embodiment
The present invention is further illustrated below in conjunction with drawings and Examples.
A kind of optoacoustic coupling spectroscopic methodology detects the device and method of food and medicine component and content fast, wherein, pick-up unit, as described in Figure 1, specifically comprising: radiation of light source unit 100, sensing chamber's unit 200, spectrum unit 300, optoacoustic detection unit 400, signal processing unit 500, signaling control unit 600 and signal display unit 700, it is characterized in that described radiation of light source unit 100 is for launching the light of certain wavelength and energy to sensing chamber's unit 200; The input end of described spectrum unit 300 is connected with the output terminal of sensing chamber unit 200, be diffracted into spectrum for the light of sensing chamber's unit 200 transmission is carried out light splitting, recycling spectral detector 305 carries out spectrographic detection reception and converts the electric signal of corresponding intensity to; The input end of described optoacoustic detection unit 400 is also connected with the output terminal of sensing chamber unit 200, for detecting the photoacoustic signal of measured matter in sensing chamber's unit 200, and converts the electric signal of corresponding optoacoustic intensity to; The input end of described signal processing unit 500 is connected with the output terminal of optoacoustic detection unit 400 with the output terminal of spectrum unit 300, carries out signal transacting for the electric signal of the reflection spectral intensity by transmission and the electric signal of reflection optoacoustic intensity; The input end of described signaling control unit 600 is connected with the output terminal of signal processing unit 500, its effect be to signal processing unit 500 process after signal carry out analyzing and processing, and send steering order by signaling control unit 600, control the operation of radiation of light source unit 100 and signal processing unit 500 respectively; The input end of described signal display unit 700 is connected with the output terminal of signaling control unit 600, for being shown in real time by the signal after signaling control unit 600 analyzing and processing, and provides the information such as measured matter type and content.
Further, described radiation of light source unit 100 comprises light source 101, collimation lens 102 and condenser lens 103 successively along optical propagation direction.Described light source 101 is formed for pulsed laser or for Halogen lamp LED adds chopper.
Light source 101 preferably one, described light source 101 is tunable wave length pulsed laser, and its wavelength output area can be ultraviolet to infrared band.Described pulsed laser is optical parametric oscillator pulsed laser; Its specification is that 532nm pumping source adjusts Q Nd:YAG; Laser output wavelength is 680 ~ 2500nm, and can be adjustable with 1-20nm interval in wavelength coverage; Whole wave band self-energy is less than or equal to 10mJ, and rushing the duration second is 10ns; Repetition frequency is that 1-20Hz is adjustable; It is adjustable in 0-100% for exporting energy; In effective wavelength range.
Light source 101 preferably two, described light source 101 is the continuous spectrum light source of wavelength coverage from ultraviolet to infrared band, as: Halogen lamp LED (Philip, MR11/12V 35W), also need in addition to configure the chopper rotated by driving stepper motor, for generation of the light-pulse generator of certain modulating frequency.
Further, described sensing chamber's unit 200 is the cuvette of quartz or glass material.
Further, described spectrum unit 300 is plane or concave reflective grating splitting system or volume holographic transmission-type grating beam splitting system.Wherein, flat reflective grating splitting system, as shown in Figure 2, is made up of entrance slit 301, collimating mirror 302, flat reflective grating, focus lamp 304 and spectral detector 305 successively along optical propagation direction; Concave reflective grating splitting system, as shown in Figure 3, is made up of entrance slit 301, concave reflective grating and spectral detector 305 successively along optical propagation direction; Volume holographic transmission-type grating beam splitting system, as shown in Figure 4, is made up of entrance slit 301, collimating mirror 302, volume holographic transmission-type grating, focus lamp 304 and spectral detector 305 successively along optical propagation direction.
Described entrance slit 301, is preferably 50-1000 μm of adjustable width slit or pin hole.
Described flat reflective grating is preferably the plane blazed grating of 600 lines/400nm; Concave reflective grating is preferably the flat holographic concave gratings S81-35 that Ningbo Yuanlu Electro Optics C. produces, and this grid stroke is 600 lines, and clear aperature is about 29.5mm, angle of diffraction about 20.9 degree, and a point optical range is about 340-850nm.It is 1200 lines/mm, blaze wavelength 550nm that volume holographic transmission-type grating 303 is preferably grid stroke, is about 80% in the diffraction efficiency at wavelength 340 and 750nm place.
The line array CCD (TCD1251UD) that described spectral detector 305 preferably adopts Toshiba Corp to produce, effective pixel number is 2700, and adjacent picture elements centre distance is 11 μm, and photosensitive area overall length is: 29.70mm, frequency of operation is 2MHz, and photoelectric transformation efficiency is greater than 92%.
Further, described optoacoustic detection unit 400 is made up of ultrasonic detector, and described ultrasonic detector is focus type or non-focusing type ultrasonic detector.Described ultrasonic detector is preferably the I1P10NF40 type ultrasonic detector that Guangzhou Doppler electronic Science and Technology Ltd. produces, and the center response frequency of ultrasonic detector is about 10.0MHz respectively.
Further, uniform application medical supersonic coupling liquid between described ultrasonic detector and sensing chamber's unit 200, and detector detecting head need with the outside wall surface keeping parallelism of sensing chamber unit 200.
Further, described spectrum unit 300 is orthogonal space structure with the position of optoacoustic detection unit 400, and its orthogonal angles is 90 degree.
Further, described signal processing unit 500 is electrically connected successively by signal amplifier 501, traffic filter 502 and signal picker 503 and forms; Described signal picker 503 for spectrum electric signal and optoacoustic electric signal being carried out sampling, quantize and encoding according to certain frequency acquisition, and converts the digital signal of respective intensities information to; Described signal amplifier 501, traffic filter 502 and signal picker 503 are hyperchannel device, and port number is no less than 2, and described signal amplifier 501 is adjustable gain voltage amplifier; Described traffic filter 502 is active low-pass filter; Described data acquisition card 503 is the data collecting card PXI/PCI-5105 of NI company.
Further, described signaling control unit 600 is made up of computing machine 601, synchronizing sequential circuit 602, radiation of light source controller 603, signal storage 604 and analysis software 605.The output terminal of described radiation of light source controller 603 is connected with the light source 101 of radiation of light source unit 100, for the laser parameter control signal that receiving computer 601 and control software design 605 send.The output terminal of described synchronizing sequential circuit 602 with in signal processing unit 500 signal amplifier 501, traffic filter 502, signal picker 503 be connected with radiation of light source controller 603, send synchronizing signal for giving above-mentioned device thus trigger these devices and keep synchronous working.Described signal storage 604 stores for the spectral digital signal that gathered by signal picker 503 and optoacoustic digital signal.
Further, described analysis software 605 comprise computer operating system, light source control software, based on the signals collecting control software design of LabVIEW and the data analysis software based on MATLAB.
Preferably, in the present embodiment, described radiation of light source unit controls software is OPPTEK V1.2.18 type laser instrument drive software; Be responsible for unbalanced pulse laser instrument, and the basic parameter of paired pulses laser instrument (as: laser instrument exports energy, pulsed frequency and wavelength etc.) is arranged;
Preferably, in the present embodiment, described data acquisition control software is virtual instrument control software design LabVIEW, is carried out the collection of control data capture card by graphic programming, and the operation such as the real-time display of photoacoustic signal and data storage;
Preferably, in the present embodiment, described data analysis software is MATLAB programming, realizes carrying out the operations such as denoising, pre-service, qualitative and content quantitative detection to the adjuvant photoacoustic data collected;
Further, described signal display unit 700 is LCD or LED graphoscope.
Meanwhile, the invention still further relates to and utilize said apparatus to carry out the method detected, concrete steps are as follows:
The first step, sample loads, that is: sample is placed in the cuvette of sensing chamber's unit 200, if sample is liquid sample, can is directly loaded in cuvette; If sample is solid sample, first can be pulverized powdering with stone roller alms bowl, be reinstalled in cuvette after evenly sieving.
Second step, the computing machine 601 in start signal control module 600 and software 605, first open laser control software, set laser parameter, as: laser instrument exports energy percentage, modulating frequency, excitation wavelength etc.
3rd step, opens the power switch of the light source 101 in radiation of light source unit 100, and after confirming that light source works is normal, click releasing the button in the control software design of radiation of light source unit, namely send light source triggering command, at this moment light source sends radiant light.
4th step, the light that light source 100 sends, incides on the sample in the cuvette of sensing chamber's unit 200 after collimation lens 102 collimates and convergent lens 103 is assembled.Now, after absorption of sample, the light of transmission or reflection enters spectrum unit 300, that is: successively through entrance slit 301, collimated by collimation lens 302, diffraction light splitting is carried out again by grating 303, by focus lamp or condenser lens 304, diffraction light is focused into band again, is more finally detected by spectral detector 305; Meanwhile, sample absorbs incident light, causes localised expansion, thus produces ultrasonic mechanical wave, i.e. photoacoustic signal, detected by the ultrasonic detector of supersonic sounding unit 400 owing to absorbing energy.Then, spectral detector and optoacoustic detector are caught and the electric signal changed, and amplify and traffic filter 502 filtering interference signals through multiple signals amplifier 501.
5th step, the computing machine 601 of start signal control module 600 and data acquisition control software, send acquisition instructions, trigger multiplexed signal sampling card 503, according to certain frequency acquisition, parallel acquisition is carried out to spectrum electric signal and optoacoustic electric signal, and be converted to corresponding digital signal; Send instruction data storage by data acquisition control software, digital signal is transmitted through GPIB-USB bus, pci bus or PXI bus, and be stored in data-carrier store and preserve.
6th step, the data analysis software of software 605 in start signal control module 600, spectral digital signal in first calling data storer 604, Signal Pretreatment program is utilized to carry out the pre-service such as denoising to spectral signal, principal component analysis (PCA) in recycling stoichiometry modeling algorithm or hereditary scheduling algorithm, find out the characteristic wavelength of measured matter.
7th step, according to the characteristic wavelength that spectroscopic methodology is determined, these characteristic wavelengths are set by the computing machine 601 in signaling control unit 600 and radiation of light source control software design, and control through radiation of light source control module 603 pulse laser that light source 101 sends this wavelength, the measured matter in sensing chamber's unit 200 cuvette is irradiated into again through collimation lens 102 and condenser lens 103, detected by optoacoustic detector 400 after ultra-sonic, amplify through signal amplifier 501 and gathered by signal picker 503 after wave filter 502 filtering, then optoacoustic amplitude or the peak-to-peak value of dissimilar and content composition measured matter is obtained.
8th step, to the optoacoustic amplitude acquired or peak-to-peak value, the principal component analysis (PCA) of chemometrics algorithm is utilized to carry out qualitative analysis, arithmetic of linearity regression is utilized to set up the correction mathematical prediction model of optoacoustic amplitude or peak-to-peak value and measured matter concentration gradients, then quantitatively detect according to the measured matter of correction mathematical prediction model to unknown content, and the component type of measured matter and content information are shown on the display of signal display unit 700.
Be the algorithm made public in Chemical Measurement and mathematical statistics field for the principal component analysis (PCA), genetic algorithm and the arithmetic of linearity regression that use in the 6th step and the 8th step, method detailed step does not repeat to set forth herein.
The present invention is not limited to above-mentioned concrete embodiment, and those of ordinary skill in the art is from above-mentioned design, and without performing creative labour, done all conversion, all drop within protection scope of the present invention.
Claims (10)
1. the food and medicine component concentration device for fast detecting of an optoacoustic coupling spectroscopic methodology, comprise radiation of light source unit (100), sensing chamber's unit (200) and signal display unit (700), characterized by further comprising spectrum unit (300), optoacoustic detection unit (400), signal processing unit (500) and signaling control unit (600), described radiation of light source unit (100), sensing chamber's unit (200) and spectrum unit (300) set gradually along optical propagation direction, the photoacoustic signal output terminal of described sensing chamber unit (200) is connected with the photoacoustic signal input end of optoacoustic detection unit (400), the electrical signal of described spectrophotometric unit (300) and optoacoustic detection unit (400) is all connected with the electric signal input end of signal processing unit (500), the signal input part of described signaling control unit (600) is connected with the signal output part of signal processing unit (500), the control signal input end of described signal display unit (700) and radiation of light source unit (100) is all connected with the control signal output terminal of signaling control unit (600).
2. the food and medicine component concentration device for fast detecting of optoacoustic coupling spectroscopic methodology according to claim 1, it is characterized in that described radiation of light source unit (100) comprises the light source (101) set gradually along optical propagation direction, collimation lens (102) and condenser lens (103), described sensing chamber unit (200) is cuvette, described optoacoustic detection unit (400) is ultrasonic detector, described signal processing unit (500) comprises signal amplifier (501), traffic filter (502) and signal picker (503), described signaling control unit (600) comprises computing machine (601), synchronizing sequential circuit (602), radiation of light source controller (603), signal storage (604) and analysis software (605), described signal display unit (700) is graphoscope, the output terminal of described signal amplifier (501) is connected with the input end of traffic filter (502), the output terminal of described traffic filter (502) is connected with the input end of signal picker (503), the output terminal of described spectrophotometric unit (300) and optoacoustic detection unit (400) is connected with the input end of signal amplifier (501) respectively, the output terminal of described computing machine (601) respectively with synchronizing sequential circuit (602), the input end of radiation of light source controller (603) and signal display unit (700) is connected, described signal storage (604) is connected with computing machine (601) respectively with analysis software (605), the output terminal of described signal picker (503) is connected with the input end of computing machine (601), the output terminal of described radiation of light source controller (603) is connected with the input end of light source (101), the output terminal of described synchronizing sequential circuit (602) respectively with signal amplifier (501), traffic filter (502), the input end of signal picker (503) and radiation of light source controller (603) is connected.
3. the food and medicine component concentration device for fast detecting of optoacoustic coupling spectroscopic methodology according to claim 1, it is characterized in that described spectrum unit (300) comprises entrance slit (301), collimating mirror (302), grating (303), focus lamp (304) and the spectral detector (305) set gradually along optical propagation direction, described grating (303) is flat reflective grating or volume holographic transmission-type grating.
4. the food and medicine component concentration device for fast detecting of optoacoustic coupling spectroscopic methodology according to claim 1, it is characterized in that described spectrum unit (300) comprises entrance slit (301), grating (303) and the spectral detector (305) set gradually along optical propagation direction, described grating (300) is concave reflective grating.
5. the food and medicine component concentration device for fast detecting of optoacoustic coupling spectroscopic methodology according to claim 1, is characterized in that described light source (101) is formed for pulsed laser or for Halogen lamp LED and chopper.
6. the food and medicine component concentration device for fast detecting of optoacoustic coupling spectroscopic methodology according to claim 1, is characterized in that described ultrasonic detector is focus type or non-focusing type ultrasonic detector.
7. the food and medicine component concentration device for fast detecting of optoacoustic coupling spectroscopic methodology according to claim 1, is characterized in that uniform application medical supersonic coupling liquid between described ultrasonic detector and sensing chamber's unit (200).
8. the food and medicine component concentration device for fast detecting of optoacoustic coupling spectroscopic methodology according to claim 1, it is characterized in that described ultrasonic detector probe need with the outside wall surface keeping parallelism of sensing chamber's unit (200).
9. the food and medicine component concentration device for fast detecting of optoacoustic coupling spectroscopic methodology according to claim 1, it is characterized in that described spectrum unit (300) is orthogonal space structure with the position of optoacoustic detection unit (400), orthogonal angles is 90 degree, described signal amplifier (501), traffic filter (502) and signal picker (503) are hyperchannel device, and port number is at least 2 tunnels.
10. the detection method of device for fast detecting according to claim 1-9, comprises the following steps:
The first step, sample loads, that is: sample is placed in cuvette, if sample is liquid sample, is directly loaded in cuvette, if sample is solid sample, is first pulverized powdering with stone roller alms bowl, reinstalls in cuvette after evenly sieving;
Second step, opens computing machine and analysis software, first opens laser control software, sets laser parameter;
3rd step, opens the power switch of light source, and after confirming that light source works is normal, click releasing the button in the control software design of radiation of light source unit, send light source triggering command, at this moment light source sends radiant light;
4th step, the light that light source sends, incide on the sample in cuvette after collimation lens collimation and convergent lens are assembled, now, after absorption of sample, the light of transmission or reflection enters spectrum unit, successively through entrance slit, collimated by collimation lens, diffraction light splitting is carried out again by grating, by focus lamp or condenser lens, diffraction light is focused into band again, finally again to be detected by spectral detector, simultaneously, sample absorbs incident light, the photoacoustic signal produced, detected by the ultrasonic detector of supersonic sounding unit, then, spectral detector and optoacoustic detector are caught and the electric signal changed, amplify and traffic filter filtering interference signals through multiple signals amplifier,
5th step, open computing machine and data acquisition control software, send acquisition instructions, trigger multiplexed signal sampling card and parallel acquisition is carried out to spectrum electric signal and optoacoustic electric signal, and be converted to digital signal, send instruction data storage by data acquisition control software, digital signal is transmitted through GPIB-USB bus, pci bus or PXI bus, and be stored in data-carrier store and preserve;
6th step, turn-on data analysis software, the spectral digital signal in first calling data storer, utilizes Signal Pretreatment program to carry out the pre-service such as denoising to spectral signal, principal component analysis (PCA) in recycling stoichiometry modeling algorithm or hereditary scheduling algorithm, find out the characteristic wavelength of measured matter;
7th step, according to the characteristic wavelength that spectroscopic methodology is determined, these characteristic wavelengths are set by computing machine and radiation of light source control software design, and control through radiation of light source control module the pulse laser that light source sends this wavelength, the measured matter in cuvette is irradiated into again through collimation lens and condenser lens, detected by optoacoustic detector, amplify through signal amplifier and gathered by signal picker after filter filtering, then obtain dissimilar optoacoustic amplitude with content composition measured matter or peak-to-peak value;
8th step, to the optoacoustic amplitude acquired or peak-to-peak value, the principal component analysis (PCA) of chemometrics algorithm is utilized to carry out qualitative analysis, arithmetic of linearity regression is utilized to set up the correction mathematical prediction model of optoacoustic amplitude or peak-to-peak value and measured matter concentration gradients, then quantitatively detect according to the measured matter of correction mathematical prediction model to unknown content, and the component type of measured matter and content information are shown over the display.
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