CN104655666A - Low field nuclear magnetic resonance detection method of edible gelatin quality - Google Patents
Low field nuclear magnetic resonance detection method of edible gelatin quality Download PDFInfo
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- CN104655666A CN104655666A CN201310594265.4A CN201310594265A CN104655666A CN 104655666 A CN104655666 A CN 104655666A CN 201310594265 A CN201310594265 A CN 201310594265A CN 104655666 A CN104655666 A CN 104655666A
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Abstract
The invention discloses a low field nuclear magnetic resonance detection method of edible gelatin quality. The method comprises the following steps: a, after edible gelatin and technical gelatin are dissolved in distilled eater according to 25% of water massic volume concentration, low field nuclear magnetic resonance detection is carried out so as to obtain low field nuclear magnetic resonance relaxation spectrum information of pure gelatin; a series of edible gelatin adulteration samples doped with different mass percentages of technical gelatin are prepared and low field nuclear magnetic resonance detection is carried out to obtain low field nuclear magnetic resonance relaxation spectrum information of each adulteration sample, and a low field nuclear magnetic resonance relaxation spectrum information database of edible gelatin is established; and b, gelatin samples to be detected undergo low field nuclear magnetic resonance detection, and obtained relaxation spectrum information and the relaxation spectrum information in the low field nuclear magnetic resonance relaxation spectrum information database of edible gelatin are analyzed and compared, and whether technical gelatin is doped in the edible gelatin to be detected is determined. The method provided by the invention has advantages of high accuracy of measuring results, good repeatability, good stability, low time consumption and the like.
Description
Technical field
The present invention relates to a kind of food additives detection method, particularly one utilizes low-field nuclear magnetic resonance profile information to differentiate edible gelatin and industrial gelatine, and detects the method that pseudo-amount mixed by industrial gelatine in edible gelatin.
Background technology
Edible gelatin is the hydrolysate of collagen, fat free high protein, is the kasher adjuvant of national regulation, is applied to various food service industry widely as jelling agent, stabilizing agent, thickening agent etc.Industrial gelatine is the gelatin utilizing the tanned useless leather of leather industry or extract for raw material from the leftover pieces that tanned leather is cut, and is wherein inevitably mingled with the impurity such as heavy metal, chemical substance, has potential harm to health.
" toxic capsule " event in 2012 and the exposure of " leather shoes Yoghourt " event then show that industrial gelatine has flowed to medicine trade and food service industry.At present, detect leather hydrolysate and listed in second batch " the non-edible material from soybeans of the illegal interpolation of possibility in food and the food additives kind list of easy abuse " by the Ministry of Public Health, whether detect it containing the foundation that can be used as the investigation judging whether to mix industrial gelatine, but detection method one hurdle of industrial gelatine is then shown as "None".
In fact, the general content by detecting heavy metal chromium in gelatin judges the quality of edible gelatin at present, and common method has atomic absorption spectrography (AAS), chemoluminescence method, electrochemical process, chromatography and mass spectroscopy etc.But these methods all more or less exist some problems, the atomic absorption spectrography (AAS) as conventional needs gelatin sample to carry out the pre-service such as high temperature ashing or micro-wave digestion, and pretreatment time generally needs more than two hours; And the method for content of 6-valence Cr ions needs to be extracted by the sexavalent chrome in sample under sour environment in the detection gelatin proposed in the patent that the patent No. is CN102841090A, then decolour, finally detect chromic content by ultraviolet spectrophotometry.These methods need use a large amount of chemical reagent, complex operation, consuming time longer.In addition, be also difficult to identify in capsule whether with the addition of industrial gelatine by means of only mensuration chromium content.Therefore, seek and differentiate that the detection method of edible/industrial gelatine seems particularly important to gelatin quality monitoring fast and effectively.
Low-field nuclear magnetic resonance (LF-NMR) is a kind of novel Dynamic Non-Destruction Measurement, mainly through the longitudinal relaxation time (T to detected object
1), T2 (T
2), coefficient of diffusion and CPMG (Carr-Purce1l-Meiboom-Gill) echo data analyze, carry out the qualitative and quantitative analysis of material, there is quick, accurate, harmless feature play a role in the analysis and research in the multiple field of food service industry, but have no the report that application low-field nuclear magnetic resonance technology carries out gelatin quartile length.
In sum, seek low-field nuclear magnetic resonance technology tool in the research of gelatin Quality Identification to be of great significance.
Summary of the invention
The object of the present invention is to provide a kind of detection method utilizing low-field nuclear magnetic resonance relaxation diagram spectrum information to differentiate edible gelatin quality.
In order to achieve the above object, present invention employs following technical scheme: a kind of low-field nuclear magnetic resonance detection method of edible gelatin quality, mainly comprises the following steps:
(1) foundation of edible gelatin low-field nuclear magnetic resonance relaxation diagram spectrum information database
Pure edible gelatin and pure industrial gelatine are dissolved in water respectively, are mixed with the solution that mass body volume concentrations is 25%, detect through low-field nuclear magnetic resonance, obtain the low-field nuclear magnetic resonance relaxation diagram spectrum information of pure edible gelatin and pure industrial gelatine; Industrial gelatine is mixed edible gelatin, be mixed with a series of standard being mixed with the industrial gelatine of different quality percentage and mix pseudo-gelatin sample, standard is mixed pseudo-gelatin sample and be dissolved in water respectively, be mixed with the solution that mass body volume concentrations is 25%, carry out low-field nuclear magnetic resonance detection respectively, obtain the low-field nuclear magnetic resonance relaxation diagram spectrum information that each standard mixes pseudo-gelatin sample, set up the low-field nuclear magnetic resonance relaxation diagram spectrum information database of edible gelatin quality;
(2) detection of edible gelatin sample to be measured
By water-soluble for edible gelatin sample to be measured, be mixed with the gelatin solution that mass body volume concentrations is 25%, detect the low-field nuclear magnetic resonance relaxation diagram spectrum information obtaining edible gelatin to be measured through low-field nuclear magnetic resonance; Profile information in the low-field nuclear magnetic resonance relaxation diagram spectrum information database of itself and edible gelatin quality being carried out com-parison and analysis, determining that whether edible gelatin to be measured is for mixing pseudo-gelatin, mixes pseudo-gelatin in this way, then that determines to mix pseudo-gelatin further mixes pseudo-mass percentage.
Described a series of standard being mixed with the industrial gelatine of different quality percentage is mixed in pseudo-gelatin sample, the mass percent mixing pseudo-industrial gelatine is 1-9% and 10-90%, and within the scope of 1-9%, percentage composition gradient is 1%, within the scope of 10-90%, percentage composition gradient is 10%.
Described low-field nuclear magnetic resonance relaxation diagram spectrum information comprises the initial time T of first peak
21, the second peak initial time T
22, the 3rd peak initial time T
23, first peak peak area percent S
21, the second peak peak area percent S
22, the 3rd peak peak area percent S
23and single component relaxation time T
2W.
The low-field nuclear magnetic resonance detection method of edible gelatin quality of the present invention has following advantage and disadvantage:
1, differentiate that speed is fast, identification result is accurate;
2, reproducible, good stability;
3, this method is limited to 1% to the lowest detection that pseudo-amount mixed by industrial gelatine in edible gelatin.
Accompanying drawing explanation
Fig. 1 is the polycomponent relaxation collection of illustrative plates of edible gelatin, industrial gelatine, gelatin to be measured;
Fig. 2 is for mixing the polycomponent relaxation collection of illustrative plates of pseudo-known industrial gelatine (0%-100%);
Fig. 3 is for mixing the T of pseudo-known industrial gelatine (0%-100%) sample
22peak initial time is with the situation of change of mixing pseudo-amount;
Fig. 4 is for mixing the S of pseudo-known industrial gelatine (0%-100%) sample
22ratio is with the situation of change of mixing pseudo-amount;
Fig. 5 is for mixing the T of pseudo-known industrial gelatine (0%-100%) sample
23peak initial time is with the situation of change of mixing pseudo-amount;
Fig. 6 is for mixing the S of pseudo-known industrial gelatine (0%-100%) sample
23ratio is with the situation of change of mixing pseudo-amount;
Fig. 7 is for mixing the polycomponent relaxation collection of illustrative plates of pseudo-industrial gelatine (0%-9%) sample;
Fig. 8 mixes the single component relaxation collection of illustrative plates of pseudo-industrial gelatine (0%-100%) sample;
Fig. 9 is for mixing the T of pseudo-industrial gelatine (0%-100%) sample
2Wwith the situation of change of mixing pseudo-amount;
Figure 10 is for mixing the single component relaxation collection of illustrative plates of pseudo-industrial gelatine (0%-9%) sample;
Embodiment
(1) preparation of gelatin solution
Take the pure edible gelatin of certain mass in beaker, add the distilled water of certain volume, wherein the mass body volume concentrations of edible gelatin and distilled water is 25%, make edible gelatin in distilled water swelling 2 hours, after swelling end, the beaker that edible gelatin is housed is placed in the thermostat water bath water-bath 15 minutes of 65 DEG C, is stirred in water-bath process, to ensure that gelatin dissolves completely.The preparation method of other gelatin solution is identical with the preparation method of this edible gelatin solution.Mixed respectively in various edible gelatins by industrial gelatine according to the pseudo-massfraction of mixing of 1%-9% and 10%-90%, the preparation of mixing the solution of pseudo-sample is identical with the preparation method of pure edible gelatin solution.
(2) foundation of edible gelatin low-field nuclear magnetic resonance relaxation information database
Get the gelatin solution 3ml prepared in (1) and move into nuclear magnetic resonance test tube, first constant temperature 10min in 32 DEG C of thermostat water baths, be placed in nuclear-magnetism probe again and stablize 1min post-sampling, sample is placed in again 32 DEG C of constant temperature 5min after sampling, to carry out sampling next time, each increment product duplicate measurements three times.The profile information recorded comprises the initial time T of first peak
21, the second peak initial time T
22, the 3rd peak initial time T
23, first peak peak area percent S
21, the second peak peak area percent S
22, the 3rd peak peak area percent S
23and single component relaxation time T
2W.These profile information and edible gelatin quality are set up correlativity, sets up edible gelatin low-field nuclear magnetic resonance relaxation information database.
1. polycomponent relaxation collection of illustrative plates (T
2, ms)
In polycomponent relaxation collection of illustrative plates, by each peak by appearance order called after T respectively
21peak, T
22peak and T
23peak.Known by Fig. 1, edible gelatin has significantly different from the relaxation collection of illustrative plates of industrial gelatine: be under the condition of 25% at mass body volume concentrations, edible gelatin has three peaks, and industrial gelatine has two peaks, and the T of industrial gelatine
22peak, T
23the relaxation time at peak is all compared with the T of edible gelatin
22peak, T
23the relaxation time at peak is short.This may be because the starting material of industrial gelatine---containing tanning agent in leather-solid waste, tanning agent is used for the tanning of rawhide, tanning effect is exactly crosslinked suturing, namely in collagen structure, new intermolecular linkage is formed, the physicochemical property of collagen are changed, and the process making gelatin is exactly destroy the intermolecular and intramolecular covalent cross-linking of stable collagenous fibres and non-covalent bond by suitable disposal route, discharge tropocollagen molecule, then make the hydrogen bond of stable collagen helix also rupture thus discharge gelatin by heating.Other impurity such as the tanning agent contained in industrial gelatine, wherein protein structure may be caused to be different from the structure of protein in edible gelatin, make individual chemical environment residing for peak in industrial gelatine that the change of a certain degree occur, finally cause the peak of industrial gelatine to be different from the peak of edible gelatin.The relaxation collection of illustrative plates of two kinds of gelatin samples to be measured has significantly different from the relaxation collection of illustrative plates of edible gelatin, industrial gelatine: there is T
21peak, T
23relaxation time at peak is compared with the T of edible gelatin
23the relaxation time at peak is short, but compared with the T of industrial gelatine
23the relaxation time at peak is long.
Industrial gelatine mixes the polycomponent relaxation collection of illustrative plates of pseudo-edible gelatin as shown in Figure 2, by each peak by appearance order called after T respectively
21peak, T
22peak and T
23peak, corresponding peak area percent (area at this peak accounts for the number percent of whole figure area under spectrum) is expressed as S
21number percent, S
22percentage is S when
23number percent.As seen from Figure 2, when to mix pseudo-amount be 40%, the T of sample
21peak disappears; Along with the increase of mixing pseudo-massfraction, mix the T of pseudo-sample
23peak departs from the T of edible gelatin
23peak, to the T of industrial gelatine
23peak is drawn close.
The Changing Pattern of the LF-NMR signal of pseudo-amount sample is mixed, by T in order to analyze difference further
22, T
23peak initial time, T
22, T
23whole T shared by peak area
2the situation of change that the number percent of figure area under spectrum mixes pseudo-massfraction with industrial gelatine lists in Fig. 3, Fig. 4, Fig. 5, Fig. 6 respectively.
Known by Fig. 3 to Fig. 6, T
22peak initial time is with mixing the change of pseudo-massfraction without evident regularity change, T
22the peak area percent S at peak
22number percent reduces with the increase of mixing pseudo-massfraction; T
23peak initial time reduces with the increase of mixing pseudo-massfraction, and becomes good binomial funtcional relationship (R
2>0.90); T
23the peak area percent S at peak
23number percent increases with the increase of mixing pseudo-massfraction, and in good linear relationship (R
2>0.90).
This industrial gelatine mixes in other edible gelatin, detects, also obtain similar result and rule, especially T through low-field nuclear magnetic resonance
23peak initial time increases and the rule of shortening with mixing pseudo-massfraction.Known by Fig. 1, the T of industrial gelatine
23peak initial time is shorter than the T of edible gelatin
23peak initial time, this is that impurity owing to not having in the edible gelatins such as the chromium in industrial gelatine makes T in industrial gelatine
23binding force suffered by Hydrogen Proton corresponding to peak is greater than T in edible gelatin
23binding force suffered by Hydrogen Proton corresponding to peak, when industrial gelatine is incorporated in edible gelatin, change the chemical environment residing for Hydrogen Proton in former edible gelatin, along with the increase of mixing pseudo-massfraction, binding force in sample suffered by Hydrogen Proton is increasing, then the T of sample
23peak initial time shortens with the increase of mixing pseudo-massfraction.
Utilize T
23peak initial time seeks the detectability that pseudo-edible gelatin mixed by industrial gelatine, as shown in Figure 7, when mixing pseudo-massfraction and being 1%, mixes the T of pseudo-sample
23the T of peak initial time and edible gelatin
23peak initial time has significant difference, and therefore lowest detection is limited to 1%.
2. one-component relaxation collection of illustrative plates (T
2W, ms)
Gelatin sample is regarded as an overall composition and carry out inverting, the one-component relaxation collection of illustrative plates that difference mixes the sample of pseudo-amount can be obtained, as shown in Figure 8.
As shown in Figure 8, with the increase of mixing pseudo-massfraction, the one-component relaxation time (T of gelatin sample
2w) reduce gradually, the T of gelatin sample
2Wvalue is with mixing the variation relation of pseudo-massfraction as shown in Figure 9.
Fig. 9 shows, the T of gelatin sample
2Wvalue shortens with the increase of mixing pseudo-massfraction, and presents good binomial funtcional relationship (R between the two
2>0.90).This is because industrial gelatine is incorporated in edible gelatin, and the chemical environment in sample residing for Hydrogen Proton is changed, and the binding force that Hydrogen Proton receives increases, the T of the reflection sample global feature finally making LF-NMR detect
2Wrelaxation behavior also there occurs change.
Utilize one-component relaxation time (T
2w) seek the detectability that pseudo-edible gelatin mixed by industrial gelatine, as shown in Figure 10, when mixing pseudo-massfraction and being 1%, mix the T of pseudo-sample
2wwith the T of edible gelatin
2whave significant difference, therefore lowest detection is limited to 1%.
Result of study shows, can continue the kind expanding edible gelatin and industrial gelatine, improve gelatin low-field nuclear magnetic resonance relaxation diagram modal data storehouse, carries out discriminating detect market not having the edible gelatin of quality guarantee.
Claims (3)
1. a low-field nuclear magnetic resonance detection method for edible gelatin quality, is characterized in that, mainly comprise the following steps:
(1) foundation of the low-field nuclear magnetic resonance relaxation diagram spectrum information database of edible gelatin quality
Pure edible gelatin and pure industrial gelatine are dissolved in water respectively, are mixed with the solution that mass body volume concentrations is 25%, detect through low-field nuclear magnetic resonance, obtain the low-field nuclear magnetic resonance relaxation diagram spectrum information of pure edible gelatin and pure industrial gelatine; Industrial gelatine is mixed edible gelatin, be mixed with a series of standard being mixed with the industrial gelatine of different quality percentage and mix pseudo-gelatin sample, standard is mixed pseudo-gelatin sample and be dissolved in water respectively, be mixed with the solution that mass body volume concentrations is 25%, carry out low-field nuclear magnetic resonance detection respectively, obtain the low-field nuclear magnetic resonance relaxation diagram spectrum information that each standard mixes pseudo-gelatin sample, set up the low-field nuclear magnetic resonance relaxation diagram spectrum information database of edible gelatin quality;
(2) detection of edible gelatin quality to be measured
By water-soluble for edible gelatin sample to be measured, be mixed with the gelatin solution that mass body volume concentrations is 25%, detect the low-field nuclear magnetic resonance relaxation diagram spectrum information obtaining edible gelatin to be measured through low-field nuclear magnetic resonance; Profile information in the low-field nuclear magnetic resonance relaxation diagram spectrum information database of itself and edible gelatin quality being carried out com-parison and analysis, determining that whether edible gelatin to be measured is for mixing pseudo-gelatin, mixes pseudo-gelatin in this way, then that determines to mix pseudo-gelatin further mixes pseudo-mass percentage.
2. the low-field nuclear magnetic resonance detection method of edible gelatin quality according to claim 1, it is characterized in that: described a series of standard being mixed with the industrial gelatine of different quality percentage is mixed in pseudo-gelatin sample, the mass percent mixing pseudo-industrial gelatine is 1-9% and 10-90%, within the scope of 1-9%, percentage composition gradient is 1%, within the scope of 10-90%, percentage composition gradient is 10%.
3. the low-field nuclear magnetic resonance detection method of edible gelatin quality according to claim 1, is characterized in that: described low-field nuclear magnetic resonance relaxation diagram spectrum information comprises the initial time T of first peak
21, the second peak initial time T
22, the 3rd peak initial time T
23, first peak peak area percent S
21, the second peak peak area percent S
22, the 3rd peak peak area percent S
23and single component relaxation time T
2W.
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| CN106770412A (en) * | 2016-11-29 | 2017-05-31 | 广东海洋大学 | A kind of rapid assay methods of gelatin Gel strength |
| CN106885816A (en) * | 2017-02-27 | 2017-06-23 | 上海海洋大学 | A kind of method of Non-Destructive Testing injecting glue aquatic products |
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Cited By (4)
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| CN105445307A (en) * | 2015-12-08 | 2016-03-30 | 大连工业大学 | Method for detecting texture quality by low field nuclear magnetic resonance in sea cucumber salting process |
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| CN106770412A (en) * | 2016-11-29 | 2017-05-31 | 广东海洋大学 | A kind of rapid assay methods of gelatin Gel strength |
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