CN110501439A - A kind of Stable isotope ratio identifies the analysis method of milk different sources - Google Patents
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Abstract
This application involves the analysis methods that foodstuff traceability identification field more particularly to a kind of Stable isotope ratio identify milk different sources.The milk sample of this method is direct or freeze-dried at powder, after grinding uniformly, measures carbon stable isotope ratio delta by elemental analysis-isotope mass spectrometer EA-IRMS13C and nitrogen Stable isotope ratio δ15N；Milk sample directly passes through the hydrogen stable isotope ratio delta in Multipurpose gas preparation-continuous flow stable isotope mass spectrograph GasBench-IRMS measurement milk water2H and oxygen stable isotope ratio delta18O；The application application above method carries out δ to the milk sample of Australia, Austria, Germany, Spain, New Zealand, Italy and China13C、δ15N、δ2H and δ18The test of O carries out diversification statistical analysis to testing result, and the discrimination model of foundation distinguishes the place of production of milk.Result of study shows the δ using milk13C、δ15N and δ2H statistical analysis has certain feasibility in milk place of production application aspect, has certain meaning to the place of production of supervision milk.
Description
Technical field
This application involves foodstuff traceability identification fields more particularly to a kind of Stable isotope ratio to identify milk different sources
Analysis method.
Background technique
Milk is liked since its is full of nutrition, easy to digest and absorb, quality-high and inexpensive, convenient by consumer.It is adjoint
The raising of living standards of the people, its consumption demand is constantly increased, it is higher and higher to its quality requirement.As China imports and exports
Trade flourishes, and the presented trend of globalization, imported product become the daily selection of domestic consumer to food trade successively
Object.The selling price of milk is irregular in existing market, the milk of same type and specification, since the difference in the place of production can
Several times even tens times of price variance can be brought, therefore the authenticity in the milk place of production is worth with extremely important determining its
Meaning.
European Union had proposed the concept in the place of production early in 1992 in terms of food authenticity, and the life of food was required in 2000
The links such as production, processing and circulation establish system of tracing to the source, and specify rule of origin, and the U.S., Japan and other countries are also established in succession and be can be traced
System, China " the law of food safety " clear stipulaties producer or marketer of food should establish Traceability system in accordance with the law, guarantee
The trackability of food.
Chinese invention patent application (publication number: CN108593829A, publication date: 2018-09-28) discloses a kind of pair of ox
The milk place of production is traced to the source the Stable Isotopic Analysis method of influence factor, includes the following steps: to acquire different lactation or different samplings
The milk sample of time measures its Stable isotope ratio after freeze-dried；If the milk sample of different lactation
It is had differences between the Stable isotope ratio, then determines lactation period to influence the factor that the milk place of production is traced to the source；If difference is adopted
It is had differences between the Stable isotope ratio of the milk sample of sample time, then determines the sampling time to influence milk
The factor that the place of production is traced to the source.Which disclose the factors that the milk place of production is traced to the source, but do not disclose discrimination model further.
Summary of the invention
In order to solve the above technical problems, the purpose of the application is to provide a kind of Stable isotope ratio and identifies milk not
With the analysis method in the place of production, this method measures the carbon of milk by elemental analysis-isotope mass spectrometer (EA-IRMS), nitrogen is stablized
Isotopic ratio (δ13C and δ15N), Multipurpose gas preparation-continuous flow stable isotope mass spectrograph (GasBench-IRMS) is surveyed
Determine the stable hydrogen and oxygen isotopes ratio (δ of water in milk2H and δ18O).With the δ of milk13C, δ15N, δ2H and δ18Tetra- indexs of O are
Object is analyzed, while the milk sample of Australia, Austria, Germany, Spain, New Zealand, Italy and China is carried out
Test and statistics compare, and the feasibility for differentiating that the milk place of production is traced to the source to it is analyzed, and propose discrimination model.
In order to achieve the above purpose, the application uses technical solution below:
A kind of Stable isotope ratio identifies the analysis method of milk different sources, which is characterized in that the milk of this method
Sample is direct or freeze-dried at powder, after grinding uniformly, measures carbon by elemental analysis-isotope mass spectrometer EA-IRMS
Stable isotope ratio δ13C and nitrogen Stable isotope ratio δ15N；Milk sample directly passes through Multipurpose gas preparation-continuous flow
Stable isotope mass spectrograph GasBench-IRMS measures the hydrogen stable isotope ratio delta in milk water2H；
Utilize δ in milk13C、δ15N and δ2The discrimination model that H combined index is established is successively:
Y(Australia)=-261.78-13.82 δ13C+25.72δ15N–0.38δ2H；
Y(Austria)=-250.32-14.53 δ13C+22.07δ15N–0.28δ2H；
Y(Germany)=-194.36-11.72 δ13C+21.80δ15N–0.07δ2H；
Y(New Zealand)=-273.18-14.54 δ13C+24.16δ15N–0.29δ2H；
Y(Spain)=-159.48-10.91 δ13C+19.25δ15N–0.17δ2H；
Y(Italy)=-165.70-10.56 δ13C+20.22δ15N–0.20δ2H；
Y(China)=-130.69-9.45 δ13C+13.59δ15N–0.48δ2H；
Wherein: Y(Australia) indicate the Australian place of production, Y(Austria)It indicatesAustriaThe place of production, Y(Germany)Indicate the German place of production, Y(New Zealand)
Indicate the New Zealand place of production, Y(Spain)Indicate the Spain place of production, Y(Italy)Indicate the Italian place of production, Y(China)Indicate China；
When carrying out identifying classification to the blind sample from different regions, the measurement result of each sample is substituted into above-mentioned differentiation respectively
Model, more each region Y value size, blind sample belong to the maximum region of Y value.
As a further improvement, the elemental analyser parameter: He flow rate of carrier gas 200mL/min, CO2With reference to gas velocity
90mL/min, oxygen gas flow rate 180mL/min aoxidize furnace temperature: 960 DEG C, restoring 640 DEG C of furnace temperature, water trap temperature 50 C.
As a further improvement, the Multipurpose gas preparing instrument GasBench parameter: H2/ He or CO2/ He gaseous mixture
Flow velocity 100mL/min, each sample purge 5min, He flow rate of carrier gas 0.5mL/min, GC chromatographic column constant temperature: 50 DEG C, sample injection disc temperature
25 DEG C of degree.
As a further improvement, the isotope ratio mass spectrometer parameter: Ionization mode: EI ion source, ion source electricity
Pressure: 3.06kV, vacuum degree: 1.2 × 10-6MBar, electric current: 1.5mA.
As a further improvement, the test equipment δ13C、δ15The METHOD FOR CONTINUOUS DETERMINATION precision < 0.06 ‰ of N, n=10；δ2H
METHOD FOR CONTINUOUS DETERMINATION precision < 0.4 ‰, n=10.
As a further improvement, each sample progress parallel testing is averaged in the analytic process, every 5 samples are worn
Insert a standard sample.
As a further improvement, the carbon stable isotope ratio delta13C and nitrogen Stable isotope ratio δ15The measurement of N
Method is as follows: taking 2 μ L milk samples to be placed in tin can, seals, enter elemental analyser by autosampler, directly progress carbon
The test of Stable isotope ratio；Milk is freeze-dried into powder, grinding uniformly, takes dry powder 0.8mg to be placed in tin can,
Sealing enters elemental analyser by autosampler, directly carries out the test of nitrogen Stable isotope ratio.
As a further improvement, the hydrogen stable isotope ratio delta2The measuring method of H is as follows: taking the milk of mixing
Platinum catalyst, sealing is added into 12mL sample bottle in 500 μ L, and sample bottle is put into autosampler, H2/He gaseous mixture is passed through
Purge mode is full of sample bottle, drives air in bottle out of；Sample bottle seals static balance 60min, so that gaseous mixture in sample bottle
2H/1H in 2H/1H and milk water reaches isotopic equilibrium；Headspace sampling is tested by GasBench-IRMS.
The application application element analysis-isotope mass spectrometer (EA-IRMS) and Multipurpose gas preparation-continuous flow are stablized same
Position quality spectrometer (GasBench-IRMS) is measured carbon, nitrogen, stable hydrogen and oxygen isotopes ratio in milk, and it is right to explore its
The feasibility of different milk place of production discriminating analyses.Milk sample directly measures carbon stable isotope ratio (δ by EA-IRMS13C) or freeze-dried at powder, after grinding uniformly, is measured by EA-IRMS and obtain nitrogen Stable isotope ratio (δ15N)。
AsBench-IRMS directly measures hydrogen and oxygen stable isotope ratio (δ in milk water2H and δ18O).Using the above method to Australia
Big Leah, Austria, Germany, Spain, New Zealand, Italy and the milk sample of China carry out δ13C、δ15N、δ2H and δ18O
Test, to testing result carry out diversification statistical analysis, the place of production of milk is distinguished.Result of study shows using milk
δ13C、δ15N and δ2H statistical analysis has certain feasibility in milk place of production application aspect, has to the place of production of supervision milk
Certain meaning.
Detailed description of the invention
Fig. 1 is the measurement spectrogram of carbon (A), nitrogen (B), hydrogen (C), oxygen (D) stable isotope.
Fig. 2 is the δ of country variant milk13C、δ15N、δ2H and δ18O test result.
Fig. 3 is milk δ13C, δ15N、δ2H and δ18The tree-like figure of O Hierarchical Clustering.
Specific embodiment
1 test portion
1.1 instruments and reagent
2000 type elemental analyser of Flash (Thermo Fisher company)；Delta/Mat 252GasBench II is more
Purposes gas preparing instrument (Thermo Fisher company)；Delta V Advantage type stable isotope mass spectrograph (Thermo
Fisher company)；2.5Triad type freeze drier (LabConco company)；CPA225D type analysis balance (is accurate to
0.01mg, Sai Duolisi scientific instrument (Beijing) Co., Ltd).Tin can (9mm × 5mm, Thermo Fisher company)；Platinum
(Pt) catalyst (Thermo Fisher company)；He gas and CO2Gas (purity >=99.999%, than Europe gas (Suzhou)
Co., Ltd)；O2Gas (purity >=99.999%, Hangzhou Deqing success gas Co., Ltd)；N2Gas (purity >=
99.999%, Biouxi Gas Industry Co., Ltd. Shanghai)；H2(purity >=99.999%, upper Hypon hydrogen industry have gas
Limit company).H2/ He gaseous mixture (H2Content 1.99%) and CO2/ He gaseous mixture (CO2Content 0.301%) (Hangzhou new century mixing
Gas Co., Ltd).Standard substance: caffeine (IAEA-600): δ13C=-27.771 ‰ ± 0.043 ‰ (VPDB) is (international former
Zi Neng mechanism)；Pidolidone (USGS40): δ13C=-26.39 ‰ ± 0.04 ‰ (VPDB-LSVEC), δ15N=-4.52 ±
0.06‰(Air N2)；Glycine (USGS65): δ13C=-20.29 ± 0.04 ‰ (VPDB-LSVEC), δ15N=20.68 ±
0.06‰(Air N2)；Water (USGS45): δ2H=-10.3 ± 0.4 ‰ (VSMOW-SLAP), δ18O=-2.238 ± 0.011 ‰
(VSMOW-SLAP), USGS47: δ2H=-150.2 ± 0.5 ‰ (VSMOW-SLAP),
δ18O=-19.80 ± 0.02 ‰ (VSMOW-SLAP), USGS50: δ2H=32.8 ± 0.4 ‰ (VSMOW-SLAP),
δ18O=4.95 ± 0.02 ‰ (VSMOW-SLAP) (United States Geological Survey), as reference gas calibration substance and matter
Amount control reference substance.Sample: Australian milk: 35 samples (12 brands)；Austrian milk: 5 sample (1 product
Board)；German milk: 9 samples (3 brands)；Spain's milk: 4 samples (1 brand)；New Zealand's milk: 13 samples
(4 brands)；Italian milk: 7 samples (2 brands)；Chinese milk: 10 samples (8 brands) supervise sample.
1.2 instrument operating conditions
Elemental analyser parameter (measurement of carbon, nitrogen stable isotope ratio): He flow rate of carrier gas 200mL/min, CO2Reference gas
Flow velocity 90mL/min, oxygen gas flow rate 180mL/min aoxidize furnace temperature: 960 DEG C, restoring 640 DEG C of furnace temperature, water trap temperature 50 C.
GasBench parameter (measurement of stable hydrogen and oxygen isotopes ratio): H2/ He or CO2/ He gaseous mixture flow velocity 100mL/min, each sample
Product purge 5min, He flow rate of carrier gas 0.5mL/min, GC chromatographic column constant temperature: 50 DEG C, 25 DEG C of sample injection disc temperature.Isotope ratio mass spectrum
Instrument parameter: Ionization mode: EI ion source, ion source voltage: 3.06kV, vacuum degree: 1.2 × 10-6MBar, electric current: 1.5mA.
Test equipment δ13C、δ15N and δ18METHOD FOR CONTINUOUS DETERMINATION precision < 0.06 ‰ (n=10) of O；δ2The METHOD FOR CONTINUOUS DETERMINATION precision of H < 0.4 ‰ (n=
10).Each sample progress parallel testing is averaged in analytic process, and every 5 samples intert a standard sample.
Stable isotope is than calculation formula: δ (‰)=(RSample/RStandard- 1) × 1000, wherein R is heavy isotope and light same position
Plain abundance ratio, i.e.,13C/12C,15N/14N,2H/1H,18O/16O.Wherein δ13The relative standard of C is V-PDB and VPDB-LSVEC, δ15N
Relative standard be air in nitrogen, δ2H and δ18The relative standard of O is VSMOW-SLAP.δ13C, δ15N, δ2H and δ18O measurement
Spectrogram is as shown in Figure 1.
Data processing carries out one-way analysis of variance, the analysis of Duncan Multiple range test, cluster to data using SPSS 20.0
Analysis and discriminant analysis.Clustering uses Hierarchical Clustering, and wherein clustering distance is Euclidean distance, and clustering method joins between using group
Connect clustering procedure.Discriminant analysis uses Fisher linear discriminant analysis.
1.3 test method
1.3.1 the measurement of carbon, nitrogen Stable isotope ratio
It takes 2 μ L milk samples to be placed in tin can, seals, elemental analyser is entered by autosampler, directly progress carbon
The test of Stable isotope ratio.Milk is freeze-dried into powder, grinding uniformly, takes dry powder 0.8mg to be placed in tin can,
Sealing enters elemental analyser by autosampler, directly carries out the test of nitrogen Stable isotope ratio.
1.3.2 the measurement of hydrogen stable isotope ratio
It takes the 500 μ L of milk of mixing into 12mL sample bottle, platinum (Pt) catalyst, sealing is added, sample bottle is put into automatically
Sample injector, by H2/ He gaseous mixture is full of sample bottle by purge mode, drives air in bottle out of.Sample bottle seals static balance
60min, so that gaseous mixture in sample bottle2H/1In H and milk water2H/1H reaches isotopic equilibrium.Headspace sampling passes through
GasBench-IRMS is tested.
1.3.3 the measurement of oxygen stable isotope ratio
It takes the 500 μ L of milk of mixing into 12mL sample bottle, sample bottle is placed in autosampler after sealing, by CO2/He
Gaseous mixture is filled with sample bottle by purge mode and drives air in bottle away.Sample bottle seals static balance 18h, makes gaseous mixture CO2's18O/16In O and milk water18O/16O reaches isotopic equilibrium state.Headspace sampling is tested by GasBench-IRMS.
2 results and discussion
The variance analysis of 2.1 carbon, nitrogen, stable hydrogen and oxygen isotopes between region
Pass through the ox to Australia, Austria, Germany, Spain, New Zealand, Italy and Chinese 7 different geographicals
Carbon, nitrogen, stable hydrogen and oxygen isotopes are detected in milk, and test result statistical conditions are as shown in Fig. 2, and carry out test result
Variance analysis, the results are shown in Table 1, δ13C value from big to small region sequence be followed successively by China and Italy > Spain > Germany >
Australia, Austria and New Zealand.The δ of country variant milk13C is different, can reflect out milk cow in raising using difference
The plant of type and different feeding manners, if with C in breeding process3Based on plant herbage, then its δ13C value is less than normal, with
C4Based on plant herbage or the auxiliary materials such as cornstalk are introduced, then its δ13C value is bigger than normal.
δ15The region sequence of the test result of N from big to small is followed successively by Australia > New Zealand, Germany > Italy, ground difficult to understand
Benefit and Spain > China, test result show import milk δ15N, which exists, is higher than domestic milk δ15The phenomenon that N.Research shows that δ15N
It is not only related with feed, also influenced by territorial environment, weather, soil regime and production method and animal own metabolism.
Therefore different geographical milk δ15N can have a certain difference.
δ2The region sequence of H test result from big to small is followed successively by Australia > New Zealand > Spain > Germany > Italy
> Austria > China, as the result is shown δ2H shows the larger situation of data area and standard deviation, the i.e. δ of milk2H is between region
There are biggish differences.Since hydrogen stable isotope composition and local drinking water are closely related, the carrier of regional information can be used as,
Therefore it can be used for the analysis of provenance.δ18The region sequence of O test result from big to small is followed successively by Australia > New Zealand
> Spain > Germany > Italy > Austria > China, δ18O and δ2The size of data sequence of H is almost the same.To δ2H and δ18O is carried out
Correlation analysis, two parameters are there are certain positive correlation, wherein different geographical δ2The test result difference of H is more apparent, because
This δ2H reflecting regional differential effect can be more significant.
The carbon of 1 country variant milk of table, nitrogen, stable hydrogen and oxygen isotopes ratio situation
Numerical value in table is mean+SD, same row difference lowercase indicate there are significant difference (p <
0.05), different capitalizations indicate that there are extremely significant sex differernce (p < 0.01).
2.2 carbon, nitrogen, stable hydrogen and oxygen isotopes index clustering
In order to tentatively judge carbon, nitrogen, stable hydrogen and oxygen isotopes ratio reflection areal variation and classifying quality, the application
Hierarchial-cluster analysis is carried out to test result.Clustering uses Hierarchical Clustering, and wherein clustering distance is Euclidean distance, cluster side
Method couples clustering procedure between using group.As shown in figure 3, arborescence is cut off from cluster 3.50, milk sample can be divided into 4 classes,
Wherein the 1st class and the 2nd class are mainly the milk of Australia and New Zealand, wherein Hispanic milk is also contained, the 3rd class master
It to be the milk of Germany and Italy, the 4th class is mainly the milk of China and Austria, wherein containing 1 Italian ox
Milk.In terms of cluster result, the measurement of stable isotope can carry out certain classification and differentiation to milk sample, can be used as milk
The reference index that the place of production differentiates.
The discriminant analysis of 2.3 carbon, nitrogen, hydrogen stable isotope index to the milk place of production
In order to further determine carbon, nitrogen, stable hydrogen and oxygen isotopes to the differentiation effect in the milk place of production, each index is understood
Effect in milk provenance, the application discriminant analysis is using Fisher linear discriminant method to the differentiation energy of different indexs
Power is compared, and the reliability of discrimination model is tested using crosscheck method (leaving-one method).From table 2 it can be seen that in area
When dividing milk region source, the differentiation effect of single index is weaker, and the whole of crosscheck differentiates that accuracy is lower than 60%, wherein
δ2H index differentiates that effect is slightly better than other indexs.It will test after parameter is combined, differentiate that accuracy is obviously improved, δ13C, δ15N
And δ2Tri- indicator combination crosschecks of H are whole to differentiate that accuracy reaches 84.3%, and wherein there are phases for Australia and New Zealand
Mutually the case where erroneous judgement.Due to δ2H and δ18There are certain correlations by O, and are introducing δ18O final finishing differentiation rate is not promoted, because
This uses δ13C, δ15N and δ2H combined index carries out discriminant analysis to the milk place of production.
Differentiation result of the 2 stable isotope index of table to the milk place of production
To δ13C、δ15N and δ2H combined index carries out discriminant function and variance contribution ratio analysis, the results show that discriminant function 1
Variance contribution ratio 88.8%, while containing δ13C、δ15N and δ2The information of H；The variance contribution ratio 8.1% of discriminant function 2, mainly
Include δ13C and δ2The information of H.The variance contribution ratio 3.1% of discriminant function 3 mainly includes δ15The information of N.Therefore speculate δ13C、
δ2H is that the milk place of production differentiates main reference index, followed by δ15N.Differentiate the result shows that, the milk sample of different geographical can be with
Certain differentiation is carried out, wherein the case where Germany and Italy are overlapped there are part milk, the milk of Australia and New Zealand
It is slightly poor that effect is distinguished in the place of production.
Utilize δ in milk13C、δ15N and δ2The discrimination model that H combined index is established is successively:
Y(Australia)=-261.78-13.82 δ13C+25.72δ15N–0.38δ2H；
Y(Austria)=-250.32-14.53 δ13C+22.07δ15N–0.28δ2H；
Y(Germany)=-194.36-11.72 δ13C+21.80δ15N–0.07δ2H；
Y(New Zealand)=-273.18-14.54 δ13C+24.16δ15N–0.29δ2H；
Y(Spain)=-159.48-10.91 δ13C+19.25δ15N–0.17δ2H；
Y(Italy)=-165.70-10.56 δ13C+20.22δ15N–0.20δ2H；
Y(China)=-130.69-9.45 δ13C+13.59δ15N–0.48δ2H；
Blind sample from different regions identify when sorting out, the measurement result of each sample can be substituted into respectively and above-mentioned be sentenced
Other model, more each region Y value size, blind sample belong to the maximum region of Y value.
The above are the descriptions to the embodiment of the present application to keep this field special by the foregoing description of the disclosed embodiments
Industry technical staff can be realized or use the application.Various modifications to these embodiments carry out those skilled in the art
Saying will be apparent.General Principle defined herein can be the case where not departing from spirit herein or range
Under, it realizes in other embodiments.Therefore, the application is not intended to be limited to these implementation columns shown in the application, but wants
Meet the widest scope consistent with principle disclosed in the present application and novel point.
Claims (8)
1. the analysis method that a kind of Stable isotope ratio identifies milk different sources, which is characterized in that the milk sample of this method
Product are direct or freeze-dried at powder, and after grinding uniformly, it is steady to measure carbon by elemental analysis-isotope mass spectrometer EA-IRMS
Determine isotopic ratio δ13C and nitrogen Stable isotope ratio δ15N；It is steady that milk sample directly passes through Multipurpose gas preparation-continuous flow
Determine the hydrogen stable isotope ratio delta in isotope mass spectrometer GasBench-IRMS measurement milk water2H；
Utilize δ in milk13C、δ15N and δ2The discrimination model that H combined index is established is successively:
Y(Australia)=-261.78-13.82 δ13C+25.72δ15N–0.38δ2H；
Y(Austria)=-250.32-14.53 δ13C+22.07δ15N–0.28δ2H；
Y(Germany)=-194.36-11.72 δ13C+21.80δ15N–0.07δ2H；
Y(New Zealand)=-273.18-14.54 δ13C+24.16δ15N–0.29δ2H；
Y(Spain)=-159.48-10.91 δ13C+19.25δ15N–0.17δ2H；
Y(Italy)=-165.70-10.56 δ13C+20.22δ15N–0.20δ2H；
Y(China)=-130.69-9.45 δ13C+13.59δ15N–0.48δ2H；
Wherein: Y(Australia) indicate the Australian place of production, Y(Austria)It indicatesAustriaThe place of production, Y(Germany)Indicate the German place of production, Y(New Zealand)It indicates
The New Zealand place of production, Y(Spain)Indicate the Spain place of production, Y(Italy)Indicate the Italian place of production, Y(China)Indicate China；
When carrying out identifying classification to the blind sample from different regions, the measurement result of each sample is substituted into above-mentioned differentiation mould respectively
Type, more each region Y value size, blind sample belong to the maximum region of Y value.
2. a kind of Stable isotope ratio according to claim 1 identifies the analysis method of milk different sources, feature
It is, elemental analyser parameter: He flow rate of carrier gas 200mL/min, CO2With reference to gas velocity 90mL/min, oxygen gas flow rate 180mL/
Min aoxidizes furnace temperature: 960 DEG C, restoring 640 DEG C of furnace temperature, water trap temperature 50 C.
3. a kind of Stable isotope ratio according to claim 1 identifies the analysis method of milk different sources, feature
It is, Multipurpose gas preparing instrument GasBench parameter: H2/ He or CO2/ He gaseous mixture flow velocity 100mL/min, each sample are blown
5min is swept, He flow rate of carrier gas 0.5mL/min, GC chromatographic column constant temperature: 50 DEG C, 25 DEG C of sample injection disc temperature.
4. a kind of Stable isotope ratio according to claim 1 identifies the analysis method of milk different sources, feature
It is, isotope ratio mass spectrometer parameter: Ionization mode: EI ion source, ion source voltage: 3.06kV, vacuum degree: 1.2 × 10- 6MBar, electric current: 1.5mA.
5. a kind of Stable isotope ratio according to claim 1 identifies the analysis method of milk different sources, feature
It is, test equipment δ13C、δ15The METHOD FOR CONTINUOUS DETERMINATION precision < 0.06 ‰ of N, n=10；δ2The METHOD FOR CONTINUOUS DETERMINATION precision < 0.4 ‰ of H, n=
10。
6. a kind of Stable isotope ratio according to claim 1 identifies the analysis method of milk different sources, feature
It is, each sample progress parallel testing is averaged in analytic process, and every 5 samples intert a standard sample.
7. a kind of Stable isotope ratio according to claim 1 identifies the analysis method of milk different sources, feature
It is, carbon stable isotope ratio delta13C and nitrogen Stable isotope ratio δ15The measuring method of N is as follows: 2 μ L milk samples being taken to set
In tin can, sealing enters elemental analyser by autosampler, directly carries out the test of carbon stable isotope ratio；It will
Milk is freeze-dried into powder, and grinding uniformly, takes dry powder 0.8mg to be placed in tin can, is sealed, is entered by autosampler
Elemental analyser directly carries out the test of nitrogen Stable isotope ratio.
8. a kind of Stable isotope ratio according to claim 1 identifies the analysis method of milk different sources, feature
It is, hydrogen stable isotope ratio delta2The measuring method of H is as follows: taking the 500 μ L of milk of mixing into 12mL sample bottle, platinum is added
Catalyst, sealing, sample bottle are put into autosampler, and H2/He gaseous mixture is full of sample bottle by purge mode, is driven out of in bottle
Air；Sample bottle seals static balance 60min, so that the 2H/1H of the gaseous mixture and 2H/1H in milk water reaches same in sample bottle
Position element balance；Headspace sampling is tested by GasBench-IRMS.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
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| CN112285192A (en) * | 2020-09-30 | 2021-01-29 | 中国肉类食品综合研究中心 | Method for identifying mutton producing area and application thereof |
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| CN112362827A (en) * | 2020-11-25 | 2021-02-12 | 上海海关动植物与食品检验检疫技术中心 | Method for tracing milk producing area |
| CN112730584A (en) * | 2021-01-18 | 2021-04-30 | 天津师范大学 | BJ-1 wheat sulfur stable isotope detection method based on sulfur monoxide mode |
| CN114088800A (en) * | 2021-11-19 | 2022-02-25 | 福建中医药大学 | Method and system for tracing production area and planting stage of ganoderma lucidum |
| CN114088800B (en) * | 2021-11-19 | 2024-02-09 | 福建中医药大学 | Method and system for tracing ganoderma lucidum production area and planting stage thereof |
| CN114324676A (en) * | 2022-03-09 | 2022-04-12 | 中国农业科学院蜜蜂研究所 | Method for identifying royal jelly produced by different food grains |
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