CN104950005A - Qualitative analysis method for distinguishing water contents of lightly dried sea cucumber, salt dried sea cucumber and expanded sea cucumber - Google Patents
Qualitative analysis method for distinguishing water contents of lightly dried sea cucumber, salt dried sea cucumber and expanded sea cucumber Download PDFInfo
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- CN104950005A CN104950005A CN201410116235.7A CN201410116235A CN104950005A CN 104950005 A CN104950005 A CN 104950005A CN 201410116235 A CN201410116235 A CN 201410116235A CN 104950005 A CN104950005 A CN 104950005A
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Abstract
The invention discloses a qualitative analysis method for distinguishing water contents of lightly dried sea cucumber, salt dried sea cucumber and expanded sea cucumber. The qualitative analysis method is applicable to identification of the lightly dried sea cucumber and the salt dried sea cucumber and rapid quality identification in a lightly dried sea cucumber expanding process. The qualitative analysis method is characterized in that nuclear magnetic resonance signals of the lightly dried sea cucumber, the salt dried sea cucumber and the expanded sea cucumber are taken as main observation objects, and a transverse relaxation time map T2 and magnetic resonance imaging of the lightly dried sea cucumber, the salt dried sea cucumber and the expanded sea cucumber are taken as a main differential basis, so that qualities of the lightly dried sea cucumber, the salt dried sea cucumber and the expanded sea cucumber are rapidly and accurately identified. The qualitative analysis method has the advantages that accuracy of a measuring result is high, short time is consumed, a sample is not damaged, visual information is provided for interior of the sample, and thus reliable information is provided for detection of dried sea cucumber and change of quality in a sea cucumber expanding process.
Description
Technical field
The invention belongs to low-field nuclear magnetic resonance sea cucumber attributional analysis field, be specifically related to a kind of method that low-field nuclear magnetic resonance differentiates sea cucumber quality.
Background technology
Unsalted dried sea cucumbers is the class dried sea-cucumber product improving due to production technology in recent years and deeply like by consumer.But some sea cucumber enterprises can occupy more weight in order to the salinity in sea cucumber body, by the process of sea cucumber salt adding boiling repeatedly, some sea cucumber salt content is up to more than 80%, and haline water is repeatedly after boiling, the nutritional labeling of sea cucumber can largely be destroyed (document 1: Liu Tianhong, Wang Lianzhu. the examination and analysb [J] of the every quality index of dried sea-cucumber. food science and technology, 2008, (8): 209-212), so differentiate that unsalted dried sea cucumbers and salt dried sea-cucumber have great importance.In addition, the large quantity research of current people to dried sea-cucumber rehydration mainly concentrates on the analysis aspect of its rehydration effect and nutritional labeling, and change little to the research of sea cucumber material properties affect about moisture distribution and state, utilize nuclear magnetic resonance technique, sea cucumber moisture distribution and state change are studied, and rise and send out physical parameter in process for the change of matter structure parameter in Holothurian machining process by detecting sea cucumber theoretical foundation (document 2: Zhang Wenjie is provided, Xue Changhu. the research [J] that low-field nuclear magnetic resonance and imaging technique change sea cucumber reconstitution process moisture state. food industry science and technology, 2012, 33 (23): 90-92).Research sea cucumber is risen, and to send out the change of quality in process be very necessary to instructing the processing technology of sea cucumber.
Nuclear magnetic resonance has been widely used in each field as a kind of important modern analysis means.According to nuclear magnetic resonance principle, specific pulse train is adopted to excite the atomic nucleus in sample with fixed magnetic moment, produce relaxation signals, this relaxation signals intensity is directly proportional to nuclear spin number contained in sample, and the constituent structure of signal attenuation process and measured matter is closely related.By mathematical method, back analysis is carried out to relaxation signals, various composition and micromechanism information that other means are difficult to obtain can be obtained, thus reach testing goal (document 3: Zhou Hang, Li Zerong, Li Baoguo. the progress [J] of nuclear magnetic resonance technique in food quality is analyzed. processing of farm products, 2009 (3): 47-49.).
Compared with differentiating sea cucumber quality method with tradition, nuclear magnetic resonance technique can keep the integrality of sample; Method of operating is simple and quick, and measurement result is accurate; Measurement result is not subject to the impact of sample of material size and appearance luster.Therefore, nuclear magnetic resonance technique is one very potential sea cucumber quality New Technique for Fast (document 4:Isabel S á nchez-Alonso, Iciar Martinez, Javier S á nchez-Valencia.Estimation of freezing storage time and quality changes in hake (Merlucciusmerluccius, L.) by low field NMR [J] .Food Chemistry, 2012:135,1626-1634).
The present invention is fully recognized that importance and the necessity of sea cucumber quartile length, and recognize the advantage of NMR (Nuclear Magnetic Resonance) relaxation time series analysis at sea cucumber quartile length, sea cucumber quality can not only improve detection speed and accuracy greatly to adopt relaxation data to differentiate, may realize real-time online simultaneously and detect.
Summary of the invention
Object of the present invention: provide a kind of low-field nuclear magnetic resonance to analyze the method for sea cucumber quality, the method not only can be differentiated unsalted dried sea cucumbers and salt dried sea-cucumber and rise to send out the change of sea cucumber quality, and detection speed is fast, accuracy is high, it is a kind of method being applicable to sea cucumber Quality Identification.
Technical scheme of the present invention: a kind of low-field nuclear magnetic resonance analyzes the method for sea cucumber quality, it is characterized in that first under identical parameter, carrying out NMR signal collection with salt dried sea-cucumber and a sea cucumber of rising to unsalted dried sea cucumbers, T2 collection of illustrative plates is utilized to analyze unsalted dried sea cucumbers and salt dried sea-cucumber, unsalted dried sea cucumbers and salt dried sea-cucumber is differentiated in conjunction with principal component analysis (PCA), the transverse relaxation data sending out sea cucumber by rising and magnetic resonance imaging are analyzed its quality, determine the correlativity of sea cucumber quality and nuclear magnetic resonance data, finally, set up a kind of method utilizing magnetic resonance to differentiate sea cucumber quality.
The invention process method is as follows:
(1) sample test analysis: arranged by cpmg sequence and transverse relaxation analysis is carried out to unsalted dried sea cucumbers and salt dried sea-cucumber and a sea cucumber of rising, and adopt the anti-Laplacian algorithm of one dimension to compose inversion algorithm as T2, draw unsalted dried sea cucumbers and salt dried sea-cucumber and rise and send out the transverse relaxation collection of illustrative plates of sea cucumber; Obtain rising by multilayer spin echo (SE) sequence and send out the T of sea cucumber
1weighted imaging and T
2weighted imaging.
(2) standard specimen reperformance test: by sending out the test analysis as described in step (1) that sea cucumber carries out repeatedly to unsalted dried sea cucumbers and salt dried sea-cucumber and rising, thus the probability understanding that magnetic nuclear resonance method judges by accident in sea cucumber Quality Identification.
(3) foundation of sea cucumber quality method is identified: according to the transverse relaxation data T of unsalted dried sea cucumbers and salt dried sea-cucumber
2analyze in conjunction with principal component analysis (PCA), obtain the major component scatter diagram of unsalted dried sea cucumbers and salt dried sea-cucumber, unsalted dried sea cucumbers and salt dried sea-cucumber are differentiated; The transverse relaxation data and magnetic resonance imaging result of sending out sea cucumber according to rising, determine to rise and send out the correlativity of sea cucumber quality and nuclear magnetic resonance data, sets up the method for qualification sea cucumber quality.
Advantage of the present invention: the method can ensure to carry out nuclear magnetic resonance spectroscopy test to sea cucumber fast and accurately, thus identifies fast sea cucumber quality, provides quality assurance for consumer and provides theoretical foundation for the processing of sea cucumber.Compared with traditional method, the inventive method not only increases detection speed, and the accuracy detected also improves greatly.
Accompanying drawing explanation
Fig. 1 is the transverse relaxation collection of illustrative plates of unsalted dried sea cucumbers and salt dried sea-cucumber;
Fig. 2 is the major component scatter diagram of unsalted dried sea cucumbers and salt dried sea-cucumber;
Fig. 3 is the transverse relaxation collection of illustrative plates of four dried sea-cucumbers;
Fig. 4 is the T of unsalted dried sea cucumbers pre-soak period
1weighted imaging and T
2weighted imaging;
Fig. 5 is the transverse relaxation collection of illustrative plates of the different rehydration number of times of unsalted dried sea cucumbers;
Fig. 6 is rehydration sea cucumber A
2changing trend diagram;
Fig. 7 is rehydration sea cucumber T
2changing trend diagram;
Fig. 8 is reconstitution rate and the T of unsalted dried sea cucumbers
23correlativity;
Fig. 9 is the T of the different rehydration number of times of unsalted dried sea cucumbers
1weighted imaging and T
2weighted imaging.
Embodiment
Embodiment 1: the magnetic resonance relaxation spectrum Analysis and Identification of light dry and salt dried sea-cucumber sample
Five unsalted dried sea cucumbers and five salt dried sea-cucumbers are bought in market, and quality is 2-3g.Adopt Mini MR-Rat magnetic resonance imaging analysis instrument, utilize multiple-pulse spin-echo sequence
(Carr-Purcell-Meiboom-Gill (CPMG) sequence), measures sea cucumber sample T2 T
2, optimum configurations is: 90 degree of pulsewidth P
1: 13 μ s, 180 degree of pulsewidth P
2: 26 μ s, repeated sampling stand-by period Tw:5000ms, analog gain RG1:15, digital gain DRG1:3, pre-amp gain PRG:1, NS:8, NECH:8000, receiver bandwidth SW:200KHz, start the controling parameters RFD:0.002ms in sampling time, time delay D L1:0.1ms, then adopts the anti-Laplacian algorithm of one dimension as T2 T
2(iterations: 1000000) draws the transverse relaxation characteristic collection of illustrative plates (Fig. 1) of each sample to inversion algorithm.The T of unsalted dried sea cucumbers as seen from Figure 1
21for 0.36ms, A
21at 60-90; The T of salt dried sea-cucumber
21for 0.26ms, A
21at 30-50.In order to illustrate that magnetic resonance method can differentiate light dry and salt dried sea-cucumber effectively further visually, the transverse relaxation data of sea cucumber sample are analyzed in conjunction with principal component analysis (PCA), as can be seen from Figure 2, magnetic resonance relaxation data can be utilized to distinguish unsalted dried sea cucumbers and salt dried sea-cucumber in conjunction with principal component analysis (PCA).
Embodiment 2: the magnetic resonance relaxation spectrum Analysis and Identification of unknown dried sea-cucumber sample
Detect the dried sea-cucumber that market is bought, adopt Mini MR-Rat magnetic resonance imaging analysis instrument, utilize cpmg sequence to arrange, measure sea cucumber sample T2 T
2, optimum configurations is: 90 degree of pulsewidth P
1: 13 μ s, 180 degree of pulsewidth P
2: 26 μ s, repeated sampling stand-by period Tw:5000ms, analog gain RG1:15, digital gain DRG1:3, pre-amp gain PRG:1, NS:8, NECH:8000, receiver bandwidth SW:200KHz, start the controling parameters RFD:0.002ms in sampling time, time delay D L1:0.1ms, then adopts the anti-Laplacian algorithm of one dimension as T2 T
2(iterations: 1000000) draws the transverse relaxation collection of illustrative plates of each sample to inversion algorithm through mass normalisation.Fig. 3 is the transverse relaxation collection of illustrative plates of four dried sea-cucumbers, A
21be respectively 1:66.63,2:64.60,3:45.22,4:42.83, can obtain 1 and 2 thus for unsalted dried sea cucumbers, 3 and 4 is salt dried sea-cucumber.
Embodiment 3: magnetic resonance relaxation spectrum monitoring unsalted dried sea cucumbers rise send out a process
1. choose a unsalted dried sea cucumbers sample, 2.714g, put into 1000mL beaker, pour about 500mL distilled water into, the water yield answers submergence to join body, soaking at room temperature 28h.Adopt Mini MR-Rat magnetic resonance imaging analysis instrument, utilize multilayer spin echo (SE) sequence, measure unsalted dried sea cucumbers sample and to rise T2 T in the process of sending out
2with magnetic resonance imaging (T
1weighted imaging and T
2weighted imaging), optimum configurations is: slices:6, FovRead:100mm, Fov Phase:100mm, slice width:2.0mm, slice gap:0.5mm, Readsize:256, Phase size:192, Average:4, T
1weighted imaging: TR:300, TE:19; T
2weighted imaging: TR:2000, TE:80.Set up the method that nuclear magnetic resonance technique identifies a sea cucumber quality that rises.Through magnetic resonance T
1weighted imaging and T
2weighted imaging (Fig. 4), result shows, sea cucumber imaging effect after immersion 24h remains unchanged substantially, and after illustrating that sea cucumber soaks 24h, moisture is substantially constant.So determine that 24 hours for the sea cucumber preferably pre-soaking time.
2. choose a unsalted dried sea cucumbers sample again, 2.192g, according to step 1 pre-soaking 24h, then sea cucumber electromagnetic oven big fire is boiled, be then adjusted to little fire, keep boiling to continue to boil 30min, then coolly to room temperature, sea cucumber sample is placed in 0-4 DEG C of distilled water, places 24h, this sends out once for rising.Repeat to boil once, micro-30min that boils, be placed in 0-4 DEG C of distilled water 24h, water yield submergence should be kept in boiling process to join body, repeat to rise and send out 7 times.Utilize magnetic resonance relaxation spectrum and magnetic resonance imaging monitoring unsalted dried sea cucumbers to rise the process of sending out, Fig. 5 is the transverse relaxation collection of illustrative plates of the different rehydration number of times of unsalted dried sea cucumbers, can find out the increase along with rehydration number of times, T
23move right, the relaxation time increases, and illustrates that water flow increases, and in sea cucumber body, free water content increases.Fig. 6 and Fig. 7 is respectively rehydration sea cucumber A
2and T
2changing trend diagram, visible in figure, T
22and A
22substantially do not change, T
23and A
23along with the increase of rehydration number of times increases gradually, the increase of free water content in mainly body is described in sea cucumber reconstitution process.Fig. 8 is reconstitution rate and the T of unsalted dried sea cucumbers
23correlativity, visible rehydration of unsalted dried sea cucumbers rate and T in figure
23there is good correlativity, coefficient R
2=0.987.Fig. 9 is the T of the different rehydration number of times of unsalted dried sea cucumbers
1weighted imaging and T
2weighted imaging, T
2weighted imaging is along with the increase of rehydration number of times, more and more brighter, T
1weighted imaging is dimmed gradually, further illustrates free water in sea cucumber body and increases, and water flow increases.Conclusion is: magnetic resonance relaxation spectrum and magnetic resonance imaging can be used for fast monitored and evaluate unsalted dried sea cucumbers rise send out a reconstitution process.
The invention discloses a kind of method that low-field nuclear magnetic resonance analyzes sea cucumber quality, be applicable to the discriminating of unsalted dried sea cucumbers and salt dried sea-cucumber and unsalted dried sea cucumbers to rise the Rapid identification of quality in the process of sending out, the method with unsalted dried sea cucumbers and salt dried sea-cucumber and rise send out sea cucumber NMR signal for main detection object, with unsalted dried sea cucumbers and salt dried sea-cucumber and rise and send out a sea cucumber T2 collection of illustrative plates T
2with magnetic resonance imaging for mainly to differentiate foundation, thus differentiate unsalted dried sea cucumbers and salt dried sea-cucumber fast and accurately and rise to send out the quality of sea cucumber.The inventive method has: measurement result accuracy is high, consuming time short, sample is not damaged, the advantage such as sampling interior visualization information, for the change of quality in the process of sending out of rising of the detection of dried sea-cucumber and sea cucumber provides reliable information.
Claims (6)
1. distinguish the light method with salt dried sea-cucumber of doing, it is characterized in that: adopt magnetic resonance imaging analysis instrument, cpmg sequence is utilized to arrange, first to sea cucumber sample under identical parameter, carry out NMR signal collection, then adopt the anti-Laplacian algorithm of one dimension to calculate T2 T according to gathered hydrogen nuclear magnetic resonance nuclear signal
2spectrogram (iterations: 10000,100000 or 1000000), if T
21(T
21for the appearance time at first left relaxation peak, come from the proton signal of Bound moisture in sea cucumber) <0.27ms or A
21(A
21for the area at first left relaxation peak, coming from the proton signal of Bound moisture in sea cucumber) <50 (relative area, without unit) is then salt dried sea-cucumber; If T
21>=0.27ms or A
21>=50 (relative area, without units) are then unsalted dried sea cucumbers.
2. method according to claim 1, is characterized in that:
Identical parameter refers to, 90 degree of pulsewidth P
1: 13 μ s, 180 degree of pulsewidth P
2: 26 μ s, repeated sampling stand-by period Tw:2000-10000ms, analog gain RG1:[10 is to 20, be integer], digital gain DRG1:[2, to 5, is integer], pre-amp gain PRG:[1,2,3], NS:4,8,16, NECH:2000-10000, receiver bandwidth SW:100,200,300KHz, start the controling parameters RFD:0.002-0.05ms in sampling time, time delay D L1:0.1-0.5ms.
3. rise and send out the method for qualitative analysis of sea cucumber water cut, it is characterized in that: adopt magnetic resonance imaging analysis instrument, utilize cpmg sequence to arrange, first under identical parameter, NMR signal collection is carried out to a sea cucumber of rising of more than 2;
Conclusion is: along with free water content in sea cucumber body increases, its T
23(T
23for the appearance time at third left relaxation peak, come from the proton signal of free water in sea cucumber) move right, the relaxation time increases, and A
23(A
23for the area at third left relaxation peak, come from the proton signal of Bound moisture in sea cucumber) increase gradually, therefore can distinguish more than 2 rise and send out the height of sea cucumber water cut.
4. method for qualitative analysis according to claim 3, is characterized in that:
Transverse relaxation data T
2condition determination be: 90 degree of pulsewidth P
1: 13 μ s, 180 degree of pulsewidth P
2: 26 μ s, repeated sampling stand-by period Tw:2000-10000ms, analog gain RG1:[10 is to 20, be integer], digital gain DRG1:[2, to 5, is integer], pre-amp gain PRG:[1,2,3], NS:4,8,16, NECH:2000-10000, receiver bandwidth SW:100,200,300KHz, start the controling parameters RFD:0.002-0.05ms in sampling time, time delay D L1:0.1-0.5ms.
5. method for qualitative analysis according to claim 3, is characterized in that:
Rise and send out a sea cucumber and refer to light dry or salt dried sea-cucumber pre-soaking 24h, then sea cucumber electromagnetic oven is boiled, keep boiling to continue to boil 10-40min, then coolly to room temperature, sea cucumber sample is placed in 0-4 DEG C of distilled water, place 20-24h, repeat to rise and send out 3-7 time;
Conclusion is: send out number of times increase, its T along with unsalted dried sea cucumbers repeats to rise
23(appearance time at third left relaxation peak comes from the proton signal of free water in sea cucumber) moves right, and the relaxation time increases, and A
23(A
23for the area at third left relaxation peak, come from the proton signal of Bound moisture in sea cucumber) increase gradually, reflect that in the process of sending out that repeats to rise, in sea cucumber body, free water content increases gradually.
6. method for qualitative analysis according to claim 3, is characterized in that:
Magnetic resonance imaging condition determination is: slices:[4-10], Fov Read:100mm, Fov Phase:100mm, slice width:2.0-3.0mm, slice gap:0.5-1mm, Read size:256, Phase size:192, Average:2,4,8, T
1weighted imaging: TR:300-500ms, TE:19-20ms; T
2weighted imaging: TR:1600-2000ms, TE:60-80ms;
Result along with rehydration number of times increase, T
2weighted imaging is more and more brighter, T
1weighted imaging is dimmed gradually, further illustrates the quality that magnetic resonance imaging can monitor a sea cucumber of rising.
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Application publication date: 20150930 |