CN102854166B - Identifying and locating method of melamine in plant protein feedstuff - Google Patents
Identifying and locating method of melamine in plant protein feedstuff Download PDFInfo
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- CN102854166B CN102854166B CN201210203760.3A CN201210203760A CN102854166B CN 102854166 B CN102854166 B CN 102854166B CN 201210203760 A CN201210203760 A CN 201210203760A CN 102854166 B CN102854166 B CN 102854166B
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- melamine
- protein feed
- vegetable protein
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- 229920000877 Melamine resin Polymers 0.000 title claims abstract description 62
- JDSHMPZPIAZGSV-UHFFFAOYSA-N melamine Chemical compound NC1=NC(N)=NC(N)=N1 JDSHMPZPIAZGSV-UHFFFAOYSA-N 0.000 title claims abstract description 62
- 238000000034 method Methods 0.000 title claims abstract description 33
- 108010064851 Plant Proteins Proteins 0.000 title abstract 8
- 235000021118 plant-derived protein Nutrition 0.000 title abstract 8
- 238000012937 correction Methods 0.000 claims abstract description 11
- 238000004458 analytical method Methods 0.000 claims abstract description 10
- 238000003384 imaging method Methods 0.000 claims abstract description 5
- 238000011282 treatment Methods 0.000 claims abstract description 5
- 244000046052 Phaseolus vulgaris Species 0.000 claims description 41
- 235000010627 Phaseolus vulgaris Nutrition 0.000 claims description 41
- 108010082495 Dietary Plant Proteins Proteins 0.000 claims description 35
- 238000001228 spectrum Methods 0.000 claims description 28
- 238000002835 absorbance Methods 0.000 claims description 23
- 108090000623 proteins and genes Proteins 0.000 claims description 12
- 102000004169 proteins and genes Human genes 0.000 claims description 12
- 238000012545 processing Methods 0.000 claims description 9
- 230000004807 localization Effects 0.000 claims description 8
- 241000196324 Embryophyta Species 0.000 claims description 7
- 238000010521 absorption reaction Methods 0.000 claims description 7
- 235000017060 Arachis glabrata Nutrition 0.000 claims description 3
- 244000105624 Arachis hypogaea Species 0.000 claims description 3
- 235000010777 Arachis hypogaea Nutrition 0.000 claims description 3
- 235000018262 Arachis monticola Nutrition 0.000 claims description 3
- 240000002791 Brassica napus Species 0.000 claims description 3
- 235000004977 Brassica sinapistrum Nutrition 0.000 claims description 3
- 229920000742 Cotton Polymers 0.000 claims description 3
- 240000008042 Zea mays Species 0.000 claims description 3
- 235000005824 Zea mays ssp. parviglumis Nutrition 0.000 claims description 3
- 235000002017 Zea mays subsp mays Nutrition 0.000 claims description 3
- 235000005822 corn Nutrition 0.000 claims description 3
- 235000012054 meals Nutrition 0.000 claims description 3
- 235000020232 peanut Nutrition 0.000 claims description 3
- 239000000843 powder Substances 0.000 claims description 3
- 238000012360 testing method Methods 0.000 abstract description 13
- 238000001514 detection method Methods 0.000 abstract description 12
- 238000002329 infrared spectrum Methods 0.000 abstract description 10
- 239000012535 impurity Substances 0.000 abstract 2
- 238000003333 near-infrared imaging Methods 0.000 description 9
- 238000010586 diagram Methods 0.000 description 6
- 230000003595 spectral effect Effects 0.000 description 6
- 239000000284 extract Substances 0.000 description 4
- 239000003153 chemical reaction reagent Substances 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 238000002156 mixing Methods 0.000 description 3
- 238000002203 pretreatment Methods 0.000 description 3
- 238000010790 dilution Methods 0.000 description 2
- 239000012895 dilution Substances 0.000 description 2
- 238000000605 extraction Methods 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000004497 NIR spectroscopy Methods 0.000 description 1
- 238000009360 aquaculture Methods 0.000 description 1
- 244000144974 aquaculture Species 0.000 description 1
- 230000006378 damage Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 235000013305 food Nutrition 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 238000010348 incorporation Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- IJGRMHOSHXDMSA-UHFFFAOYSA-N nitrogen Substances N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 230000035515 penetration Effects 0.000 description 1
- 238000000053 physical method Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 230000035945 sensitivity Effects 0.000 description 1
- 238000004611 spectroscopical analysis Methods 0.000 description 1
- -1 triazines nitrogen heterocyclic ring organic compound Chemical class 0.000 description 1
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- Investigating Or Analysing Materials By Optical Means (AREA)
Abstract
The invention belongs to the technical field of feedstuff detection, and discloses an identifying and locating method of melamine in a plant protein feedstuff. The method comprises the steps that: a near-infrared image of a plant protein feedstuff sample requiring testing is collected; a baseline correction treatment is carried out upon the near-infrared image of the plant protein feedstuff sample requiring testing; near-infrared spectrum characteristics of melamine and near-infrared spectrum characteristics of a plant protein feedstuff with no impurity are collected; according to the near-infrared spectrum characteristics of melamine and the near-infrared spectrum characteristics of a plant protein feedstuff with no impurity, the plant protein feedstuff sample requiring testing is subjected to characteristic wavelength imaging analysis; and weather melamine exists in the plant protein feedstuff sample requiring testing is determined, and melamine is located. The method provided by the invention has the advantages of no contact, no pollution, high detection speed, and accurate detection result.
Description
Technical field
The invention belongs to feed detection technique field, relate in particular to a kind of identification and localization method of vegetable protein Determination of Melamine in feed.
Background technology
Vegetable protein feed is a kind of important feed, and its raw material is to ensure feed quality and safe prerequisite.Yet melamine event in recent years, causes safely great threat to protein feed, the detection of melamine in protein feed is received much concern.Carry out the research work of the aspects such as the melamine detection side science of law, meet feeding quality security control in the urgent need to, for ensureing feed safety, animal food safety and body health of people, promote the healthy and sustainable development of aquaculture, and even the equal tool of maintaining social stability is of great significance.
At present, although the method sensitivity of conventional detection Determination of Melamine in feed is higher, but still exist pretreatment process complexity, complex steps and testing process to use a large amount of chemical reagent to problems such as environments.Near infrared imaging analysis combines traditional optical imagery and near infrared spectroscopy method, can obtain spatial information and the spectral information of sample simultaneously, select one as plane, can obtain the intensity response (absorbance) of all spatial point of sample under a certain specific wavelength, i.e. spectrum picture.The advantages such as sample strong without sample pre-treatments, penetration capacity, that adapt to rough surface and noncontact, non-destruction that near infrared imaging technology has.In addition, because near infrared imaging can obtain the near infrared spectrum on several microns of spaces, in to the analysis of micro substance, can avoid the problem of sample composition dilution in near-infrared spectrum analysis, and can position the object detecting, therefore the context of detection at foreign peoples's material has huge advantage.
The near infrared light spectrum signature of melamine is obvious, especially at 6900-6450cm
-1in wave-number range, have notable difference with the spectral signature of vegetable protein feedstuff, this is the spectroscopy foundation of near infrared imaging technology for detection vegetable protein Determination of Melamine in feed.
By patent documentation, periodicals and magazines and other documents of publishing are retrieved, the present invention has no report at home and abroad, does not openly use at home.
Summary of the invention
The object of the invention is to, a kind of identification and localization method of vegetable protein Determination of Melamine in feed is provided, the problem existing for solving the method for existing detection vegetable protein Determination of Melamine in feed.
For achieving the above object, technical scheme provided by the invention is that a kind of identification of vegetable protein Determination of Melamine in feed and localization method, is characterized in that described method comprises:
Step 1: the near-infrared image that gathers vegetable protein feed sample to be measured;
Step 2: the near-infrared image for the treatment of measuring plants protein feed sample carries out baseline correction processing;
Step 3: gather the near infrared light spectrum signature of melamine and the near infrared light spectrum signature of pure vegetable protein feed;
Step 4: according to the near infrared light spectrum signature of the near infrared light spectrum signature of melamine and pure vegetable protein feed, treat measuring plants protein feed sample and carry out characteristic wavelength imaging analysis, judge whether vegetable protein feed sample to be measured contains melamine and contained melamine is positioned.
Described vegetable protein feed is dregs of beans, cotton dregs, rapeseed dregs, peanut meal or corn protein powder.
The described near-infrared image for the treatment of measuring plants protein feed sample carries out baseline correction processing and specifically uses 6100-6200cm
-1the absorption value at wave number place is carried out baseline correction as benchmark.
Described step 4 is specifically:
(1) select 6900-6450cm
-1the wave number of absorbance difference maximum in the near infrared light spectrum signature of melamine and the near infrared light spectrum signature of pure vegetable protein feed in wave-number range;
(2) obtain vegetable protein feed sample to be measured at the image at the wave number place of described absorbance difference maximum;
(3) judge whether vegetable protein feed sample to be measured exists absorbance to be greater than the point of setting threshold in the image at the wave number place of described absorbance difference maximum, if vegetable protein feed sample to be measured exists absorbance to be greater than the point of setting threshold in the image at the wave number place of described absorbance difference maximum, in vegetable protein feed sample to be measured, containing the corresponding position of point that melamine and described absorbance be greater than setting threshold is the position at melamine place.
The wave number of described absorbance difference maximum is 6805cm
-1.
Described setting threshold is 0.06.
The present invention adopts pure physical method to detect in vegetable protein feed whether contain melamine, without loaded down with trivial details pre-treatment step, in processing procedure, without using chemical reagent, avoids pollution on the environment in testing process; Use simultaneously this method in testing process without testing tool contact sample, without destroying testing sample, there is detection speed fast, the feature such as testing result is accurate.
Accompanying drawing explanation
Fig. 1 is identification and the localization method process flow diagram of vegetable protein Determination of Melamine in feed;
Fig. 2 is the near infrared spectrum characteristic pattern of melamine and pure dregs of beans;
Fig. 3 is the testing result schematic diagram of dregs of beans sample to be measured; Wherein, (a) being the near infrared figure of dregs of beans sample to be measured, is (b) that dregs of beans sample to be measured is at 6805cm
-1the image at wave number place is (c) that dregs of beans sample to be measured is at 6805cm
-1in the image at wave number place, high brightness point extracts and location schematic diagram, is (d) the near infrared light spectrogram that is judged as three high brightness points extractions of melamine in Fig. 3 (c).
Embodiment
Below in conjunction with accompanying drawing, preferred embodiment is elaborated.Should be emphasized that, following explanation is only exemplary, rather than in order to limit the scope of the invention and to apply.
The present embodiment be take dregs of beans as vegetable protein feed, and implementation process of the present invention is described.
Fig. 1 is identification and the localization method process flow diagram of vegetable protein Determination of Melamine in feed.As shown in Figure 1, in dregs of beans, the identification of melamine and localization method comprise:
Step 1: the near-infrared image that gathers dregs of beans sample to be measured.
Take polytetrafluoroethylstandard standard blank as background, use near infrared imaging instrument, adopt diffuse reflection mode to gather the near-infrared image of dregs of beans sample to be measured, spectral resolution is 32cm
-1, spatial resolution is 25 μ m * 25 μ m, pixel scanning times is 8 times, interferometer index glass speed 1cm/s.
Dregs of beans sample to be measured is for being added with the dregs of beans potpourri of melamine.Before gathering near-infrared image, first adopt feed link to carry out even hybrid processing with mixing apparatus or small-size laboratory mixing apparatus, if do not possess relevant device, also can adopt the method for operating manually mixing to mix, incorporation time is not less than 1 minute, to guarantee that dregs of beans sample to be measured has sufficiently high homogeneity.
Step 2: the near-infrared image of dregs of beans sample to be measured is carried out to baseline correction processing.
When carrying out baseline correction processing, conventionally using and do not exist the absorption value at obvious absorption wavenumber place to carry out baseline correction as benchmark.The present embodiment is used 6100-6200cm
-1the absorption value at wave number place is carried out baseline correction as benchmark.
Step 3: gather the near infrared light spectrum signature of melamine and the near infrared light spectrum signature of pure dregs of beans.
While gathering the near infrared light spectrum signature of melamine, first take polytetrafluoroethylstandard standard blank as background, use near infrared imaging instrument, gather the near-infrared image of melamine, and then extract its different in nature spectral signature, obtain the near infrared light spectrum signature of melamine.Equally, while gathering the near infrared light spectrum signature of pure dregs of beans, first take polytetrafluoroethylstandard standard blank as background, use near infrared imaging instrument, gather the near-infrared image of pure dregs of beans, and then extract its different in nature spectral signature, obtain the near infrared light spectrum signature of pure dregs of beans.The near infrared light spectrum signature of the melamine collecting and the near infrared light spectrum signature of pure dregs of beans are as shown in Figure 2.
Step 4: according to the near infrared light spectrum signature of the near infrared light spectrum signature of melamine and pure dregs of beans, dregs of beans sample to be measured is carried out to characteristic wavelength imaging analysis, judge whether dregs of beans sample to be measured contains melamine and contained melamine is positioned.
(1) select 6900-6450cm
-1the wave number of absorbance difference maximum in the near infrared light spectrum signature of melamine and the near infrared light spectrum signature of pure dregs of beans in wave-number range.
The near infrared light spectrum signature of melamine is at 6900-6450cm
-1in wave-number range, there is notable difference with the near infrared light spectrum signature of vegetable protein feed.Especially, in Fig. 2 at wave number 6805cm
-1near, the near infrared light spectrum signature absorbance difference of the near infrared light spectrum signature of melamine and pure dregs of beans is especially obvious.This is because melamine is a kind of triazines nitrogen heterocyclic ring organic compound, at wave number 6805cm
-1there is responsive absorption peak in place, has reflected that N-H combination absorbs frequently, and dregs of beans at this wave number place without obvious absorption peaks.According to Fig. 2, choose wave number 6805cm
-1wave number for absorbance difference maximum.
(2) obtain dregs of beans sample to be measured at 6805cm
-1the image at wave number place.
Fig. 3 is the testing result schematic diagram of dregs of beans sample to be measured.In the present embodiment, the near-infrared image gatherer process through step 1, has obtained Fig. 3 (a), i.e. the near infrared figure of dregs of beans sample to be measured.To this figure at wave number 6805cm
-1process, obtain Fig. 3 (b), dregs of beans sample to be measured is at 6805cm
-1the image at wave number place.In Fig. 3, Micrometers is micron, and Abs is absorbance.
(3) judge that dregs of beans sample to be measured is at 6805cm
-1in the image at wave number place, whether exist absorbance to be greater than the point of setting threshold, if dregs of beans sample to be measured is at 6805cm
-1in the image at wave number place, exist absorbance to be greater than the point of setting threshold, in dregs of beans sample to be measured, containing the corresponding position of point that melamine and this absorbance be greater than setting threshold is the position at melamine place.
Utilize 6805cm
-1wave number place near infrared spectrum feature difference, can carry out characteristic wavelength imaging analysis to dregs of beans sample to be measured, observes dregs of beans sample to be measured at wave number 6805cm
-1the image at place, at the absorbance at this wave number place, determines whether dregs of beans sample to be measured contains melamine and contained melamine is positioned according to each pixel in this image.Fig. 3 (b) is that dregs of beans sample to be measured is at 6805cm
-1the image at wave number place, observation Fig. 3 (b), finds the pixel that in figure, absorbance is high (highlighted spot or punctation), shows to contain melamine in dregs of beans sample to be measured, and can position according to its locus.Otherwise in dregs of beans sample to be measured, do not contain melamine.Conventionally, absorbance is greater than 0.06 point and thinks the point that contains melamine.Through above-mentioned, the high point of absorbance in Fig. 3 (b) extracted and located, obtaining Fig. 3 (c), dregs of beans sample to be measured is at 6805cm
-1in the image at wave number place, high brightness point extracts and location schematic diagram.Fig. 3 (d) is the near infrared light spectrogram that is judged as three high brightness points extractions of melamine in Fig. 3 (c).
The present invention detects seldom measuring melamine in dregs of beans, and content can be detected is the melamine in 0.1% sample.The present invention is equally applicable to the detection of melamine in other vegetable protein feedstuffs such as cotton dregs, rapeseed dregs, peanut meal, corn protein powder.
The present invention carries out near infrared imaging to vegetable protein feed sample, and according to specificity spectral signature, carry out identification and the location of melamine, whole testing process, without sample pre-treatments, is polluted without chemical reagent, and detecting step is quick, easy, harmless, green.In addition, near infrared imaging can obtain the near infrared spectrum in several microns of spaces, in to the analysis of micro substance, can avoid the problem of sample composition dilution in near-infrared spectrum analysis, and can carry out location, locus to the object detecting.
The above; be only the present invention's embodiment preferably, but protection scope of the present invention is not limited to this, is anyly familiar with in technical scope that those skilled in the art disclose in the present invention; the variation that can expect easily or replacement, within all should being encompassed in protection scope of the present invention.Therefore, protection scope of the present invention should be as the criterion with the protection domain of claim.
Claims (4)
1. the identification of vegetable protein Determination of Melamine in feed and a localization method, is characterized in that described method comprises:
Step 1: the near-infrared image that gathers vegetable protein feed sample to be measured;
Before gathering near-infrared image, treat measuring plants protein feed sample and carry out even hybrid processing;
Step 2: the near-infrared image for the treatment of measuring plants protein feed sample carries out baseline correction processing;
Step 3: gather the near infrared light spectrum signature of melamine and the near infrared light spectrum signature of pure vegetable protein feed;
Step 4: according to the near infrared light spectrum signature of the near infrared light spectrum signature of melamine and pure vegetable protein feed, treat measuring plants protein feed sample and carry out characteristic wavelength imaging analysis, judge whether vegetable protein feed sample to be measured contains melamine and contained melamine is positioned; Specifically:
(1) select wave number 6805cm
-1;
(2) obtain vegetable protein feed sample to be measured at the image at described wave number place;
(3) judge whether vegetable protein feed sample to be measured exists absorbance to be greater than the point of setting threshold in the image at described wave number place, if vegetable protein feed sample to be measured exists absorbance to be greater than the point of setting threshold in the image at described wave number place, in vegetable protein feed sample to be measured, containing the corresponding position of point that melamine and described absorbance be greater than setting threshold is the position at melamine place.
2. method according to claim 1, is characterized in that described vegetable protein feed is dregs of beans, cotton dregs, rapeseed dregs, peanut meal or corn protein powder.
3. method according to claim 1 and 2, the near-infrared image for the treatment of measuring plants protein feed sample described in it is characterized in that carries out baseline correction processing and specifically uses 6100-6200cm
-1the absorption value at wave number place is carried out baseline correction as benchmark.
4. method according to claim 3, is characterized in that described setting threshold is 0.06.
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| CN103245632B (en) * | 2013-05-15 | 2015-06-03 | 河北科技大学 | Method for detecting nitrogen-containing compounds in liquid milk through mid-infrared spectroscopy |
| CN105067561A (en) * | 2015-08-13 | 2015-11-18 | 浙江大学 | Method for measuring content of manganese element in cotton seed meal |
| CN109709065A (en) * | 2019-02-28 | 2019-05-03 | 中国农业大学 | The method of discrimination of antibiotic bacterium dregs in a kind of cotton dregs based on near-infrared micro-imaging technique |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102243171A (en) * | 2011-04-13 | 2011-11-16 | 北京农产品质量检测与农田环境监测技术研究中心 | Method for detecting lime substances in flour with near-infrared micro-imaging technology |
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| US6734962B2 (en) * | 2000-10-13 | 2004-05-11 | Chemimage Corporation | Near infrared chemical imaging microscope |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102243171A (en) * | 2011-04-13 | 2011-11-16 | 北京农产品质量检测与农田环境监测技术研究中心 | Method for detecting lime substances in flour with near-infrared micro-imaging technology |
Non-Patent Citations (4)
| Title |
|---|
| potential of Raman spectroscopy and imaging methods for rapid and routine screening of the presence of melamine in animal feed and foods;Yongliang Liu等;《applied spectroscopy》;20090430;第63卷(第4期);全文 * |
| Yongliang Liu等.potential of Raman spectroscopy and imaging methods for rapid and routine screening of the presence of melamine in animal feed and foods.《applied spectroscopy》.2009,第63卷(第4期),第477-480页. |
| 利用纤维红外吸收特性的皮棉杂质检测新方法;郏东耀等;《红外与毫米波学报》;20050430;第24卷(第2期);第148页右栏第21-26行，第149页左栏倒数第4-6行，右栏第11-12行 * |
| 郏东耀等.利用纤维红外吸收特性的皮棉杂质检测新方法.《红外与毫米波学报》.2005,第24卷(第2期),第147-150页. |
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