CN105806872A - Method for identifying different sturgeon roes by low field nuclear magnetism technology - Google Patents
Method for identifying different sturgeon roes by low field nuclear magnetism technology Download PDFInfo
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- CN105806872A CN105806872A CN201610280882.0A CN201610280882A CN105806872A CN 105806872 A CN105806872 A CN 105806872A CN 201610280882 A CN201610280882 A CN 201610280882A CN 105806872 A CN105806872 A CN 105806872A
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- acipenser sinensis
- ovum
- sinensis ovum
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- sturgeon
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N24/00—Investigating or analyzing materials by the use of nuclear magnetic resonance, electron paramagnetic resonance or other spin effects
- G01N24/08—Investigating or analyzing materials by the use of nuclear magnetic resonance, electron paramagnetic resonance or other spin effects by using nuclear magnetic resonance
Abstract
The invention provides a method for identifying different sturgeon roes by a low field nuclear magnetism technology. The method comprises the following steps of collecting a plurality of 2-3.5mm different sturgeon roes as detecting samples in spring and autumn; performing low field nuclear magnetic resonance analysis on each sturgeon roe sample to obtain echo attenuationcurve data of sturgeon roe sample; performing principal component analysis on the obtained echo attenuation curve data, and building different sturgeon roe identifying models; performing low field nuclear magnetic resonance analysis on sturgeon roes to be tested by the same procedure as the second step, and identifying the varieties of the sturgeon roes to be tested by combining the sturgeon roe identifying models obtained in the third step. The method for identifying different sturgeon roes by the low field nuclear magnetism technology has the advantages that the great significance is realized in the aspects of reinforcing the trading circulation link technology supervision, protecting the sustainable development of Chinese special seafood product industry and improving the competitiveness of the Chinese seafood product in the international market; the method belongs to a very potential fast identifying new technology.
Description
Technical field
The present invention relates to substance classes and distinguish field, it particularly relates to utilize the method that low field nuclear-magnetism technology differentiates different Acipenser Sinensis ovum.
Background technology
Acipenser Sinensis fish roe is a kind of nutritious food, wherein there are the mineral such as substantial amounts of protein, cholesterol, vitamin, riboflavin, cephalin and calcium, phosphorus, ferrum, it is the good complement agent of human brain and bone marrow, grows agent, especially upgrowth and development of children is particularly important, but be our ordinary meal is easier lack.Carry out pickling and fermenting with the salt pair Acipenser Sinensis ovum of 2%～5%, form the caviar sold on market.Fish roe extended shelf-life after salt adding is pickled, the nutrient composition content such as moisture therein, oils and fats, protein also changes.And for different types of Acipenser Sinensis ovum, its market price, nutritive value also can be very different.But consumer is difficult to distinguish against naked eyes the kind of Acipenser Sinensis ovum.Therefore develop and differentiate the marine product technology such as Acipenser Sinensis ovum quickly, accurately, easily, for strengthening the supervision of trade flows link technology, the characteristic marine product industry sustainable development of protection China, improves China's marine product competitiveness in the international market and is of great importance.
The detection method being presently used for different Acipenser Sinensis ovum mainly includes subjective appreciation, physico-chemical process, molecular biology method and spectroscopic method.Subjective appreciation and physico-chemical process detection speed are slow, and by the impact of subjective factors so that it is it is restricted in quickly detection application.And molecular biology and spectroscopic method to there is detection method numerous and diverse, the defect such as complex steps.
Summary of the invention
Presently commercially available Acipenser Sinensis ovum product variety is various, very different, it is an object of the invention to provide a kind of method simple, quick, accurate, environmental protection different Acipenser Sinensis ovum are differentiated, utilize low-field nuclear magnetic resonance technology to differentiate pickled/not pickled Acipenser Sinensis ovum, siberia platform fish roe/Hai Borui Acipenser Sinensis ovum etc..
For reaching above-mentioned purpose, the invention provides a kind of method utilizing low field nuclear-magnetism technology to differentiate different Acipenser Sinensis ovum, comprise the steps:
S1, point spring and autumn gather and some are sized to the different Acipenser Sinensis ovum of 2～3.5 millimeters as detection sample；
S2, each Acipenser Sinensis ovum sample that step S1 is obtained carry out low-field nuclear magnetic resonance analysis, utilize CPMG pulse sequence method to gather nmr echo signal, obtain the echo attenutation curve data of each Acipenser Sinensis ovum sample；
The parameter that described CPMG pulse sequence method adopts is: 90 degree of pulsewidth P1:13 μ s, 180 degree of pulsewidth P2:26 μ s, repeated sampling waiting time Tw:1000-10000ms, analog gain RG1:[10 to 20, be integer], digital gain DRG1:[2 to 5, it is integer], pre-amp gain PRG:[1,2,3], NS:4,8,16, NECH:1000-10000, receiver bandwidth SW:100,200,300KHz, start the control parameter RFD:0.002-0.05ms, time delay D L1:0.1-0.5ms in sampling time；
S3, utilization chemometrics method, the echo attenutation curve data of the Acipenser Sinensis ovum samples that step S2 is obtained by employing TheUnscrambler statistical analysis software carries out principal component analysis, sets up different Acipenser Sinensis ovum and distinguishes model；
S4, take Acipenser Sinensis ovum 1g to be measured, adopt the program identical with step S2 that described Acipenser Sinensis ovum to be measured is carried out low-field nuclear magnetic resonance analysis, obtain the echo attenutation curve data of described Acipenser Sinensis ovum to be measured；The echo attenutation curve data of the Acipenser Sinensis ovum described to be measured obtained is carried out principal component analysis, and the Acipenser Sinensis ovum that integrating step S3 obtains distinguishes model, differentiates the kind of Acipenser Sinensis ovum to be measured.
Under optimal way, described Acipenser Sinensis ovum gathers from 6～11 Acipenser Sinensiss.
Under optimum way, described different Acipenser Sinensis ovum are Hai Borui Acipenser Sinensis ovum and siberia platform fish roe；
Under optimum way, described different Acipenser Sinensis ovum are through the pickled Acipenser Sinensis ovum of saline that over-richness is 3～5wt% with without pickled Acipenser Sinensis ovum.
Screening according to collecting sample, the present invention can realize the discriminating for pickled/not pickled Acipenser Sinensis ovum, for the discriminating of the Acipenser Sinensis ovum of variety classes Acipenser Sinensis；It is preferred that, the present invention differentiates while can realizing many difference such as pickled/not pickled, variety classes Acipenser Sinensis simultaneously.
The invention have benefit that:
1, the detection method operating process that the present invention relates to is simple, and Acipenser Sinensis ovum sample, without pre-treatment, does not need to consume organic reagent, and reproducible, analysis time is short, to Acipenser Sinensis ovum without destruction, can different Acipenser Sinensis ovum be made a distinction for non-intrusion measurement method.
2, the present invention utilizes low-field nuclear magnetic resonance technology in conjunction with principal component analysis (PCA) is qualitative, different Acipenser Sinensis ovum to be differentiated, different from traditional detection method, without sample is carried out special pre-treatment before low-field nuclear magnetic resonance detection, in detection process consuming time short, there is feature convenient, quick, accurate, pollution-free, non-invasive, unlimited by differentiating sample surfaces state (such as color, shape etc.) impact；And the inventive method can realize the multifactorial discriminating such as pickled situation, Acipenser Sinensis ovum kind simultaneously.
3, the pickled nutritional labeling that can destroy Acipenser Sinensis ovum, has the longer shelf-life than without pickled Acipenser Sinensis ovum, it is simple to transport.The inventive method can effectively realize the discriminating of pickled/not pickled Acipenser Sinensis ovum; identify through pickled and good open date can be provided out to judge for consumer person without pickled Acipenser Sinensis ovum; allow the Acipenser Sinensis ovum that explicit consumer buys whether through pickled processing, protect consumer rights.
4, current, detection method for different Acipenser Sinensis ovum mainly includes subjective appreciation, physico-chemical process etc., and these methods are capable of the differentiation of different Acipenser Sinensis ovum, but detection speed is slow, and by the impact of subjective factors, ordinary consumer is difficult to be distinguished by said method the kind of Acipenser Sinensis ovum.For siberia platform fish roe and Hai Borui Acipenser Sinensis ovum, the biochemical composition difference all to some extent of two kinds of Acipenser Sinensis ovum nutrient composition contents and coelomic fluid, thus, the market price is also different；The inventive method can realize the quick discriminating of siberia platform fish roe/Hai Borui Acipenser Sinensis ovum.Provide safeguard for consumer, it is to avoid the situation mixed the genuine with the fictitious in consumption market occurs.
In sum; the present invention utilizes the method that low field nuclear-magnetism technology differentiates different Acipenser Sinensis ovum; for strengthening the supervision of trade flows link technology; the characteristic marine product industry sustainable development of protection China; improve China's marine product competitiveness in the international market to be of great importance, be the very potential quick differentiation new technique of one.
Accompanying drawing explanation
Pickled and the not pickled Acipenser Sinensis ovum CPMG attenuation curve of Fig. 1；
Fig. 2 pickled and not pickled Acipenser Sinensis ovum main constituent scatterplot (CPMG sequence)；
Fig. 3 variety classes Acipenser Sinensis ovum CPMG attenuation curve；
Fig. 4 variety classes Acipenser Sinensis ovum main constituent scatterplot (CPMG sequence).
Detailed description of the invention
Below in conjunction with drawings and Examples, the specific embodiment of the present invention is described in more details, so as to the advantage being more fully understood that the solution of the present invention and its various aspects.Specific embodiments described below and embodiment are only descriptive purposes, rather than limitation of the present invention.
Material used in following embodiment, reagent etc., if no special instructions, all commercially obtain.
Embodiment 1
Whether Acipenser Sinensis ovum is by the method for pickled processing, comprises the steps: to utilize low field nuclear-magnetism technology to differentiate
S1, collection spring and autumn Hai Borui Acipenser Sinensis, take its diameter Acipenser Sinensis ovum between 2.5 to 3 millimeters.Wherein, not pickled Hai Borui Acipenser Sinensis ovum sample picks up from 6 Hai Borui Acipenser Sinensiss, and every fish gathers three samples, amounting to 18 samples, pickled Hai Borui Acipenser Sinensis ovum sample picks up from 11 Hai Borui Acipenser Sinensiss, and every fish gathers three samples, amounting to 33 samples, each sample takes 1g；
As detection sample, above-mentioned sample has certain representativeness.
nullS2、Each Acipenser Sinensis ovum sample that step S1 is obtained carries out low-field nuclear magnetic resonance analysis: utilize CPMG pulse sequence method to gather nmr echo signal，Adopt MiniMR-Rat magnetic resonance imaging analysis instrument that above-mentioned all Acipenser Sinensis ovum samples are carried out low field nmr analysis，Utilize CPMG pulse sequence，Measure Acipenser Sinensis ovum T2 T2，Parameter is set to: 90 degree of pulsewidth P1:13 μ s，180 degree of pulsewidth P2:26 μ s，Repeated sampling waiting time Tw:2000ms，Analog gain RG1:20，Digital gain DRG1:1，Pre-amp gain PRG:3，NS:8，NECH:6000，Receiver bandwidth SW:200KHz，Start the control parameter RFD:0.008ms in sampling time，Time delay D L1:0.2ms，Obtain echo attenutation curve.As it is shown in figure 1, obtain the echo attenutation curve data of pickled and not pickled Hai Borui Acipenser Sinensis ovum sample；
S3, utilization chemometrics method, in conjunction with TheUnscrambler software, the echo attenutation curve data of each Acipenser Sinensis ovum sample that step S2 is obtained carries out principal component analysis, whether sets up Acipenser Sinensis ovum by pickled differentiation model, Origin software is utilized to draw, as shown in Figure 2；
S4, unknown Acipenser Sinensis ovum sample differentiate: take Acipenser Sinensis ovum sample 1 to be measured, each 1g of sample 2, carry out above-mentioned steps, differentiate that whether Acipenser Sinensis ovum to be measured is pickled.Result is as in figure 2 it is shown, sample 1 is not pickled Hai Borui Acipenser Sinensis ovum, and sample 2 is pickled Hai Borui Acipenser Sinensis ovum.
Embodiment 2
The method utilizing low field nuclear-magnetism technology to differentiate Acipenser Sinensis ovum kind, comprises the steps:
R1, collection spring and autumn Hai Borui Acipenser Sinensis, take its diameter Acipenser Sinensis ovum between 2.5 to 3 millimeters, wherein, not pickled Hai Borui Acipenser Sinensis ovum sample picks up from 6 Hai Borui Acipenser Sinensiss, and every fish gathers three samples, amounts to 18 samples, not pickled siberia platform fish roe sample picks up from 6 Acipenser baeris, every fish gathers three samples, amounts to 18 samples, and each sample takes 1g；
As detection sample, above-mentioned sample has certain representativeness.
nullR2、Each Acipenser Sinensis ovum sample that step R1 is obtained carries out low-field nuclear magnetic resonance analysis: utilize CPMG pulse sequence method to gather nmr echo signal，Adopt MiniMR-Rat magnetic resonance imaging analysis instrument that above-mentioned all Acipenser Sinensis ovum samples are carried out low field nmr analysis，Utilize CPMG pulse sequence，Measure Acipenser Sinensis ovum T2 T2，Parameter is set to: 90 degree of pulsewidth P1:13 μ s，180 degree of pulsewidth P2:26 μ s，Repeated sampling waiting time Tw:2000ms，Analog gain RG1:20，Digital gain DRG1:1，Pre-amp gain PRG:3，NS:8，NECH:6000，Receiver bandwidth SW:200KHz，Start the control parameter RFD:0.008ms in sampling time，Time delay D L1:0.2ms，Obtain echo attenutation curve.As it is shown on figure 3, obtain not pickled Hai Borui Acipenser Sinensis ovum and the echo attenutation curve data of not pickled siberia platform fish roe sample；
R3, utilization chemometrics method, in conjunction with TheUnscrambler software, the echo attenutation curve data of each Acipenser Sinensis ovum sample that step R2 is obtained carries out principal component analysis, whether sets up Acipenser Sinensis ovum by pickled differentiation model, Origin software is utilized to draw, as shown in Figure 4；
R4, unknown Acipenser Sinensis ovum sample differentiate: take Acipenser Sinensis ovum sample 3 to be measured, each 1g of sample 4, carry out above-mentioned steps, differentiate the kind of Acipenser Sinensis ovum to be measured.As shown in Figure 4, sample 3 is siberia platform fish roe to result, and sample 4 is Hai Borui Acipenser Sinensis ovum.
The present invention is not only limited to pickled Hai Borui Acipenser Sinensis ovum and not pickled Hai Borui Acipenser Sinensis ovum, and the discriminating of not pickled Hai Borui Acipenser Sinensis ovum and not pickled siberia platform fish roe.
To sum up, low field nuclear-magnetism is utilized can well different Acipenser Sinensis ovum to be made a distinction in conjunction with PCA, to Acipenser Sinensis ovum sample to be measured without destruction, easy and simple to handle, detection speed can be improved.
The above; it is only the present invention preferably detailed description of the invention; but protection scope of the present invention is not limited thereto; any those familiar with the art is in the technical scope of present disclosure; it is equal to replacement according to technical scheme and inventive concept thereof or is changed, all should be encompassed within protection scope of the present invention.
Claims (4)
1. one kind utilizes the method that low field nuclear-magnetism technology differentiates different Acipenser Sinensis ovum, it is characterised in that comprise the steps:
S1, point spring and autumn gather and some are sized to the different Acipenser Sinensis ovum of 2～3.5 millimeters as detection sample；
S2, each Acipenser Sinensis ovum sample that step S1 is obtained carry out low-field nuclear magnetic resonance analysis, utilize CPMG pulse sequence method to gather nmr echo signal, obtain the echo attenutation curve data of each Acipenser Sinensis ovum sample；
The parameter that described CPMG pulse sequence method adopts is: 90 degree of pulsewidth P1:13 μ s, 180 degree of pulsewidth P2:26 μ s, repeated sampling waiting time Tw:1000-10000ms, analog gain RG1:[10 to 20, be integer], digital gain DRG1:[2 to 5, it is integer], pre-amp gain PRG:[1,2,3], NS:4,8,16, NECH:1000-10000, receiver bandwidth SW:100,200,300KHz, start the control parameter RFD:0.002-0.05ms, time delay D L1:0.1-0.5ms in sampling time；
S3, utilization chemometrics method, the echo attenutation curve data of the Acipenser Sinensis ovum samples that step S2 is obtained by employing TheUnscrambler statistical analysis software carries out principal component analysis, sets up different Acipenser Sinensis ovum and distinguishes model；
S4, take Acipenser Sinensis ovum 1g to be measured, adopt the program identical with step S2 that described Acipenser Sinensis ovum to be measured is carried out low-field nuclear magnetic resonance analysis, obtain the echo attenutation curve data of described Acipenser Sinensis ovum to be measured；The echo attenutation curve data of the Acipenser Sinensis ovum described to be measured obtained is carried out principal component analysis, and the Acipenser Sinensis ovum that integrating step S3 obtains distinguishes model, differentiates the kind of Acipenser Sinensis ovum to be measured.
2. utilize the method that low field nuclear-magnetism technology differentiates different Acipenser Sinensis ovum according to claim 1, it is characterised in that described Acipenser Sinensis ovum gathers from 6～11 Acipenser Sinensiss.
3. the method utilizing low field nuclear-magnetism technology to differentiate different Acipenser Sinensis ovum according to claim 1 or claim 2, it is characterised in that described different Acipenser Sinensis ovum are Hai Borui Acipenser Sinensis ovum and siberia platform fish roe.
4. the method utilizing low field nuclear-magnetism technology to differentiate different Acipenser Sinensis ovum according to claim 1 or claim 2, it is characterised in that described different Acipenser Sinensis ovum are through the pickled Acipenser Sinensis ovum of saline that over-richness is 3～5wt% with without pickled Acipenser Sinensis ovum.
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| CN108445035A (en) * | 2018-04-25 | 2018-08-24 | 中国农业大学 | A method of corn monoploid seed is differentiated based on nuclear magnetic resonance CPMG attenuation curves |
| CN112285144A (en) * | 2020-10-15 | 2021-01-29 | 青岛农业大学 | Method for detecting breast myopathy of white feather broiler chicken by using low-field nuclear magnetic resonance |
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