CN105301089B - A kind of Strontium Isotopic Ratios measured in strawberry tree different parts sample and the method for identifying the red bayberry place of production - Google Patents
A kind of Strontium Isotopic Ratios measured in strawberry tree different parts sample and the method for identifying the red bayberry place of production Download PDFInfo
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Abstract
The invention discloses a kind of Strontium Isotopic Ratios measured in strawberry tree different parts sample and the methods for identifying the red bayberry place of production：It weighs strawberry tree different parts sample and carries out pre-treatment, after micro-wave digestion, purified with strontium specific resin, afford strontium sample, then detect to obtain the Strontium Isotopic Ratios of strontium sample using hot surface ionization mass spectrometer.Can correlation distribution map be done according to the isotopic ratio of the strontium of the sample of different sources same area, for identifying the place of production situation of the strawberry tree sample in the unknown place of production.The present invention quickly measures the Strontium Isotopic Ratios of strawberry tree different parts sample using hot surface ionization mass spectrometer for the first time, the ratio is one kind " natural fingerprint " of strawberry tree, do not change with the change of chemical addition agent, it can trace to the source for red bayberry and a kind of science is provided, independent, identity authentication information unmodifiable and with the flowing of entire food chain, method are reliable and stable.Especially for the product between extensive area, its difference can be effectively distinguished.
Description
Technical field
The present invention relates to the technical fields of analytical chemistry, and in particular to a kind of strontium measured in strawberry tree different parts sample
Isotopic ratio and the method for identifying the red bayberry place of production.
Background technology
The globalization of food products market and food safety affair take place frequently, and increase the public attention degree of food place of production mark,
Consumer is caused increasingly to pay close attention to food sources.The trackability of food is studied, corresponding food tracing system is established and is to ensure that
One important means of food security.Place of production tracing technology is also widely used to move/derived food is planted, such as water fruits and vegetables, paddy
Class, milk, meat etc..
Place of production tracing technology is mainly the specific index for seeking characterization different geographical source food, including isotopic content
With ratio, constituent content, chemical composition content, animal genetic map, microorganism collection of illustrative plates, organoleptic attribute, volatile ingredient etc..Its
In, isotopic ratio has been found to be effective technology means that the food place of production is traced to the source.
In nature, organism constantly experience carries out physics, chemistry, Biochemical processes, such as evaporate with external environment
With condense, crystallize and dissolve, absorption and desorption, diffusion and thermal diffusion etc..These processes all can cause isotope to be fractionated (certain naturally
The measurable variation of " weight " isotope and " light " isotopic ratio of kind element).For example,13C/12C and the photosynthesis of plant way
Diameter is related,15N/14N and soil environment and agricultural fertilizer are closely related,18O/16O and2H/1H and the close phase of environmental condition of region
It closes,87Sr/86Sr, Pb and geological conditions are closely related.Therefore, the measure of natural isotopic abundance can provide plant " class first
Type " (C, N isotopic ratio) and region source (isotopic ratios such as H, O, Sr).The composition difference of isotope carry environment because
The information of son reflects the environmental condition residing for organism.And caused by this species diversity is exactly the natural fractionation effect of isotope, because
This, isotope nature fractionation effect just can be as the basic principle and foundation of tracing technology as it.Isotopics are biologies
One kind " natural fingerprint " of body, and not changing with the change of chemical addition agent, can be provided for foodstuff traceability a kind of science, solely
Identity authentication information that is vertical, unmodifiable and being flowed with entire food chain.
The commonly used target isotope of agricultural product tracing technology influences organism and environment including C, N, H, O, S and Si etc.
The isotope abundance reason of changes of middle difference element is also different.In addition to this, S and Sr elements also more should in recent years
Agricultural product have been used to trace to the source in research, the same geological environment of composition of S isotopes in soil, rainfall and with the factors such as the distance of ocean
Correlation, and stable isotope87Sr be by87Rb element decays, Sr isotopics and local geology ring in agricultural product
Border, rock age and composition are closely bound up, with regional isotope element finger print feature, Sr isotopics climate, season
Etc. external factor influence it is smaller, therefore differentiate effect it is more satisfactory.
Invention content
The present invention provides a kind of strontium isotope measured in strawberry tree different parts sample aiming at the above-mentioned state of the art
Ratio and the method for identifying the red bayberry place of production.
The technical solution adopted by the present invention is：
A kind of Strontium Isotopic Ratios measured in strawberry tree different parts sample and the method for identifying the red bayberry place of production, the side
Method includes the following steps：
(1) Strontium Isotopic Ratios of strawberry tree different parts sample are measured：
(A) sample pre-treatments：Strawberry tree different parts sample is weighed, the strawberry tree different parts sample includes red bayberry sample
Product, strawberry tree Leaf samples or strawberry tree root soil sample, are then respectively adding digestive reagent, obtain mixing sample a, b or
C is respectively placed in microwave dissolver and is cleared up, and the temperature program for setting microwave dissolver is：5min is raised to 400w, keeps
5min, then 5min rise to 800w, keep 5min, cooling down to room temperature, the heating of gained mixed liquor is evaporated, molten with 3mol/L nitric acid
It is centrifuged after solution, it is spare to respectively obtain digestion solution a, b or c；
It is described to weigh strawberry tree different parts sample, digestive reagent is separately added into, mixing sample a, b or c is obtained, specifically presses
It operates below：
(a) red bayberry sample is weighed, adds in concentrated nitric acid, obtains mixing sample a, the volumetric usage of the concentrated nitric acid is with red bayberry sample
The quality of product is calculated as 10mL/g；
(b) weigh strawberry tree Leaf samples, add in concentrated nitric acid, obtain mixing sample b, the volumetric usage of the concentrated nitric acid with
The quality of strawberry tree Leaf samples is calculated as 18mL/g；
(c) strawberry tree root soil sample is weighed, it is 5 to add in volume ratio：1 chloroazotic acid and the mix acid liquor of hydrofluoric acid, obtain
To mixing sample c, the volumetric usage of the mix acid liquor is calculated as 40mL/g with the quality of strawberry tree root soil sample；
(B) sample purification：By strontium specific resin wet method dress post, pillar is alternately cleaned 2~3 times with the nitric acid and water of 1+1, so
Afterwards successively with the nitric acid of 1+1,6mol/L hydrochloric acid and washing column, then the nitric acid balance pillar with 3mol/L, step (A) is taken to make respectively
Standby digestion solution a, b or c upper prop is first eluted with 3mol/L nitric acid, then elutes strontium with 0.03mol/L nitric acid, collects strontium eluent
It in polytetrafluoroethylene (PTFE) sample dissolving cup, heats and is evaporated on electric hot plate, respectively obtain strontium sample a, b, c；
(C) isotopic ratio of strontium is measured using hot surface ionization mass spectrometer：
(C-1) pretreatment of sample band
Rhenium band is first put into immersion 30min~60min in ethyl alcohol, after taking-up is dried, rhenium band is spoted weld on sample introduction stent,
Degassing in device of air is subsequently placed in, the rhenium band pre-processed；
(C-2) the painting sample of strontium
The tantalum pentafluoride cast charge that 1 μ L are pipetted with micropipettor is added on the rhenium band center of pretreatment, and energization is evaporated, will walk
Suddenly strontium sample a, b or c that prepared by (B) are dissolved respectively with the nitric acid of mass fraction 3%, are then put at the tantalum pentafluoride of rhenium band,
Energization is evaporated, and 1 μ L tantalum pentafluoride cast charges are added dropwise at sample, and energization is evaporated, energization reddening sample band, then by sample introduction branch
It is rack-mounted enter hot surface ionization mass spectrometer sample disc；
(C-3) the mass spectrum isotopic ratio detection of strontium
Hot surface ionization mass spectrometer vacuumizes, and vacuum degree reaches 3 × 10-7During Pa, rhenium band is heated, is tested, it will be warm
At 1500 ± 50 DEG C, detection obtains the isotopic ratio of strontium for degree control87Sr/86Sr；
(2) the Strontium Isotopic Ratios identification red bayberry place of production is utilized
According to the method for step (1), the sample of the strawberry tree different parts of different sources is taken to measure the isotope of strontium respectively
Ratio takes the isotopic ratio of the strontium of the sample of different sources same area to do correlation distribution map, available for identifying unknown production
The place of production situation of the strawberry tree sample on ground.
In the step (A), red bayberry sample, strawberry tree Leaf samples or strawberry tree root soil sample are respectively by poplar
It after plum, red bayberry leaf or the drying of strawberry tree root soil, is cut small, then is ground with mortar obtained with ceramic scissors.
The strawberry tree root soil generally takes the soil of root 5~20cm depths, preferably takes root 10cm depths
Soil.
In the step (A), the microwave dissolver is preferably using the Multiwave3000 microwaves of Anton Paar company production
Clear up instrument.
In the step (B), the nitric acid of the 1+1 is by concentrated nitric acid and water by volume 1：1 mixed preparing obtains.
In the step (B), the strontium specific resin is preferably the SR Resin-B resins of Trskem companies production.
In the step (B), after eluting strontium with 0.03mol/L nitric acid, generally require cleaning and live again pillar, the cleaning weight
The step of raw pillar is：Successively with 6mol/L hydrochloric acid, the nitric acid of 1+1 and washing column.
Further, preferred steps (B) operate by the following method：
By strontium specific resin wet method dress post, pillar is alternately cleaned 2~3 times with the nitric acid and water of 1+1, then successively with 5 times
The washing column of the nitric acid of the 1+1 of column volume, the 6mol/L hydrochloric acid of 10 times of column volumes and 10 times of column volumes, then with 5 times of column volumes
The nitric acid balance pillar of 3mol/L, digestion solution a, b or c upper prop that step (A) is taken to prepare respectively, first with 15 times of column volumes
3mol/L nitric acid elutes, then elutes strontium with the 0.03mol/L nitric acid of 12.5 times of column volumes, collects strontium eluent in polytetrafluoroethylene (PTFE)
Sample dissolving cup is heated on electric hot plate and is evaporated, and respectively obtains strontium sample a, b, c；Again successively with the 6mol/L hydrochloric acid of 10 times of column volumes,
The water of the nitric acid of the 1+1 of 10 times of column volumes and 10 times of column volumes cleans pillar of living again；
In the step (C-1), go device of air that mass spectrum filament can be used and remove device of air, degassing can be used successively with 1A and 4A
Each degassing 15min of electric current, the rhenium band pre-processed.
In the step (C-2), the tantalum pentafluoride cast charge is prepared in the following proportions：0.02g tantalic chlorides are weighed in poly-
In tetrafluoroethene sample dissolving cup, 300 μ L water are added in, makes its hydrolysis, 20 μ L hydrofluoric acid, 20 μ L concentrated phosphoric acid (quality is sequentially added after 2h
Score 85%), 200 μ L concentrated nitric acids and 800 μ L water, the heating on electric hot plate that closes the lid makes it dissolve and balance, be made described in
Tantalum pentafluoride cast charge.
The hot surface ionization mass spectrometer that the step (C) uses is preferably Thermo Triton Plus mass spectrographs.
Further, the step (C-2) preferably presses following operation：
The tantalum pentafluoride cast charge that 1 μ L are pipetted with micropipettor is added on the rhenium band center of pretreatment, and energization 0.8A is evaporated,
Strontium sample a, b or c prepared by step (B) is dissolved respectively with the nitric acid of mass fraction 3%, then puts five fluorine in rhenium band respectively
To change at tantalum, energization is evaporated, and 1 μ L tantalum pentafluoride cast charges are added dropwise at sample, and energization is evaporated, energization 2.2A reddening sample bands,
Then sample introduction stent is packed into the sample disc of hot surface ionization mass spectrometer.
When the step (C) measures the isotopic ratio of strontium using hot surface ionization mass spectrometer, generally marked using SRM987
Sample judges the reliability of the reliability of detection and method as Quality Control sample, this is well known to those skilled in the art.
The present invention also provides a kind of method for measuring the Strontium Isotopic Ratios in strawberry tree different parts sample, the methods
Include the following steps：
(A) sample pre-treatments：Strawberry tree different parts sample is weighed, the strawberry tree different parts sample includes red bayberry sample
Product, strawberry tree Leaf samples or strawberry tree root soil sample, are then respectively adding digestive reagent, obtain mixing sample a, b or
C is respectively placed in microwave dissolver and is cleared up, and the temperature program for setting microwave dissolver is：5min is raised to 400w, keeps
5min, then 5min rise to 800w, keep 5min, cooling down to room temperature, the heating of gained mixed liquor is evaporated, molten with 3mol/L nitric acid
It is centrifuged after solution, it is spare to respectively obtain digestion solution a, b or c；
It is described to weigh strawberry tree different parts sample, digestive reagent is separately added into, mixing sample a, b or c is obtained, specifically presses
It operates below：
(a) red bayberry sample is weighed, adds in concentrated nitric acid, obtains mixing sample a, the volumetric usage of the concentrated nitric acid is with red bayberry sample
The quality of product is calculated as 10mL/g；
(b) weigh strawberry tree Leaf samples, add in concentrated nitric acid, obtain mixing sample b, the volumetric usage of the concentrated nitric acid with
The quality of strawberry tree Leaf samples is calculated as 18mL/g；
(c) strawberry tree root soil sample is weighed, it is 5 to add in volume ratio：1 chloroazotic acid and the mix acid liquor of hydrofluoric acid, obtain
To mixing sample c, the volumetric usage of the mix acid liquor is calculated as 40mL/g with the quality of strawberry tree root soil sample；
(B) sample purification：By strontium specific resin wet method dress post, pillar is alternately cleaned 2~3 times with the nitric acid and water of 1+1, so
Afterwards successively with the nitric acid of 1+1,6mol/L hydrochloric acid and washing column, then the nitric acid balance pillar with 3mol/L, step (A) is taken to make respectively
Standby digestion solution a, b or c upper prop is first eluted with 3mol/L nitric acid, then elutes strontium with 0.03mol/L nitric acid, collects strontium eluent
It in polytetrafluoroethylene (PTFE) sample dissolving cup, heats and is evaporated on electric hot plate, respectively obtain strontium sample a, b, c；
(C) isotopic ratio of strontium is measured using hot surface ionization mass spectrometer：
(C-1) pretreatment of sample band
Rhenium band is first put into immersion 30min~60min in ethyl alcohol, after taking-up is dried, rhenium band is spoted weld on sample introduction stent,
Degassing in device of air is subsequently placed in, the rhenium band pre-processed；
(C-2) the painting sample of strontium
The tantalum pentafluoride cast charge that 1 μ L are pipetted with micropipettor is added on the rhenium band center of pretreatment, and energization is evaporated, will walk
Suddenly strontium sample a, b or c that prepared by (B) are dissolved respectively with the nitric acid of mass fraction 3%, are then put at the tantalum pentafluoride of rhenium band,
Energization is evaporated, and 1 μ L tantalum pentafluoride cast charges are added dropwise at sample, and energization is evaporated, energization reddening sample band, then by sample introduction branch
It is rack-mounted enter hot surface ionization mass spectrometer sample disc；
(C-3) the mass spectrum isotopic ratio detection of strontium
Hot surface ionization mass spectrometer vacuumizes, and vacuum degree reaches 3 × 10-7During Pa, rhenium band is heated, is tested, it will be warm
At 1500 ± 50 DEG C, detection obtains the isotopic ratio of strontium for degree control87Sr/86Sr。
Compared with prior art, it is as follows the advantages of the method for the present invention：
The present invention quickly measures the strontium isotope ratio of strawberry tree different parts sample using hot surface ionization mass spectrometer for the first time
Value, which is one kind " natural fingerprint " of strawberry tree, and does not change with the change of chemical addition agent, can trace to the source and carry for red bayberry
Independent for a kind of science, unmodifiable and with the identity authentication information that entire food chain flows, method is reliably steady
It is fixed.Especially for the product between extensive area, its difference can be effectively distinguished.The method of the present invention is used in pretreatment process
Acid is few, environmental protection；It crosses that the column time is short, can realize the quick separating of strontium element, detection efficiency is high；Before the method for the present invention passes through sample
Processing, matrix influence is small, and interference is few, and testing result precision is high, and effect is good.
Description of the drawings
The correlation distribution map of the Strontium Isotopic Ratios of Fig. 1 different sources red bayberry samples.
Specific embodiment
Technical scheme of the present invention is described in further detail with reference to embodiments, but protection scope of the present invention is not
It is limited to this.
The measure of the Strontium Isotopic Ratios of 1 Cixi place of production strawberry tree different parts sample of embodiment
Red bayberry sample, strawberry tree Leaf samples strawberry tree root soil sample are respectively by red bayberry, red bayberry leaf or poplar
It after the drying of Japanese apricot root soil, is cut small, then is ground with mortar obtained with ceramic scissors.
(1) 1g red bayberry samples are weighed respectively, add in 10mL concentrated nitric acids；0.5g Leaf samples add in 9mL concentrated nitric acids；0.3g
The pedotheque of red bayberry usage tree root 10cm depths adds in 10mL chloroazotic acid and 2mL hydrofluoric acid；Then it is respectively put into microwave dissolver
It is cleared up in (Multiwave3000 of Anton Paar company production), temperature program is raised to 400w for 5min, keeps 5min, then
5min rises to 800w, keeps 5min, cooling down to room temperature.After the completion of resolution, mixing liquid is transferred to 15mL polytetrafluoroethylene (PTFE)
Sample dissolving cup is positioned over 150 DEG C of heating on electric hot plate and is evaporated, and is centrifuged after being dissolved with 1mL3mol/L nitric acid, it is spare to obtain digestion solution.
(2) by strontium specific resin SR Resin-B (Trskem companies produce, 100-150 μm of grain size) wet method dress post, each
Pillar fills the resin of 200ul volumes.Pillar is alternately cleaned with the nitric acid and water of 1+1 3 times, then successively with 1mL1+1 nitric acid,
2mL6mol/L hydrochloric acid and 2mL washing columns, 1mL3mol/L nitric acid balance pillar, the digestion solution sample 0.5mL that step (1) is taken to prepare
Upper pillar is eluted with 3mL3mol/L nitric acid, 2.5mL0.03mol/L nitric acid elution strontium, then uses 2mL6mol/L hydrochloric acid successively,
Column is washed in 2mL1+1 nitric acid and 2mL water reuse (treatments.The strontium eluent eluted with 2.5mL0.03mol/L nitric acid is collected in 3mL polytetrafluoroethyl-nes
In alkene sample dissolving cup, it is placed on electric hot plate and is evaporated for 150 DEG C, it is spare to obtain strontium sample.
(3) hot surface ionization mass spectrometer (Thermo Triton Plus mass spectrographs) measures Strontium Isotopic Ratios
The pretreatment of sample band
First rhenium band is put into ethyl alcohol and impregnates 40min, after taking-up is dried, rhenium band is spoted weld on sample introduction stent, is then put
It is gone in device of air (Beijing Yi Guanjing instrument Science and Technology Ltd.) in mass spectrum filament, successively with each degassing 15min of the electric current of 1A and 4A,
The rhenium band pre-processed.
The painting sample of strontium
With the strontium sample of the generation of the nitric acid dissolving step (2) of mass fraction 3%, five fluorine of 1uL are pipetted with micropipettor
Change tantalum cast charge in the rhenium band center of pretreatment, energization 0.8A is evaporated, then again by dissolved strontium sampling point in five fluorine of rhenium band
Change at tantalum, energization is evaporated, and 1 μ L tantalum pentafluoride cast charges are added dropwise on strontium sample, and be powered after being evaporated the 2.2A reddening samples that are powered again
Then sample introduction stent is packed into the sample disc of hot surface ionization mass spectrometer by product band.
The tantalum pentafluoride cast charge is prepared by the following method：0.02g tantalic chlorides are weighed in polytetrafluoroethylene (PTFE) sample dissolving cup,
300 μ L water are added in, make its hydrolysis, it is dense that 20 μ L hydrofluoric acid, 20 μ L concentrated phosphoric acids (mass fraction 85%), 200 μ L are sequentially added after 2h
Nitric acid (mass fraction 65%) and 800 μ L water, the heating on electric hot plate that closes the lid make it dissolve and balance, five fluorine are made
Change tantalum cast charge.
The mass spectrum isotopic ratio detection of strontium
Hot surface ionization mass spectrometer vacuumizes, and treats mass spectrograph normal operation, and vacuum degree reaches 3 × 10-7When, rhenium band is added
Temperature is tested, and temperature is controlled at 1500 ± 50 DEG C, measures the isotopic ratio of strontium.
Acquired results see the table below 1
Table 1：
Embodiment 2
Take Cixi, Yuyao, three, Wenzhou place of production red bayberry sample, according to embodiment 1 method and step measure strontium same position
Plain ratio (87Sr/86Sr), correlation distribution map is done, as shown in Figure 1, Fig. 1 can be seen that the red bayberry sample in Wenzhou place of production87Sr/86Sr is than Distribution value significantly lower than Cixi and Yuyao place of production87Sr/86Sr ratios, significant difference.And Cixi, Yuyao
The place of production since region is too near,87Sr/86The difference of Sr ratios is smaller.But Fig. 1 can be used for differentiating the red bayberry in Wenzhou place of production.To not
Know the red bayberry sample in the place of production, test it87Sr/86Sr values, if numerical value can be accredited as close to the lower zone of Wenzhou sample
Wenzhou place of production, if the upper area close to Cixi and Yuyao place of production, needs further to differentiate with reference to other means.
Claims (9)
1. a kind of Strontium Isotopic Ratios measured in strawberry tree different parts sample the and method of identifying the red bayberry place of production, feature exist
In the described method comprises the following steps：
(1) Strontium Isotopic Ratios of strawberry tree different parts sample are measured：
(A) sample pre-treatments：Weigh strawberry tree different parts sample, the strawberry tree different parts sample include red bayberry sample,
Strawberry tree Leaf samples or strawberry tree root soil sample, are then respectively adding digestive reagent, obtain mixing sample a, b or c, point
It is not placed in microwave dissolver and is cleared up, the temperature program for setting microwave dissolver is：5min is raised to 400w, keeps 5min,
5min rises to 800w again, keeps 5min, cooling down to room temperature, the heating of gained mixed liquor is evaporated, after being dissolved with 3mol/L nitric acid
Centrifugation, it is spare to respectively obtain digestion solution a, b or c；
It is described to weigh strawberry tree different parts sample, digestive reagent is separately added into, mixing sample a, b or c are obtained, specifically by following
Operation：
(a) red bayberry sample is weighed, adds in concentrated nitric acid, obtains mixing sample a, the volumetric usage of the concentrated nitric acid is with red bayberry sample
Quality is calculated as 10mL/g；
(b) strawberry tree Leaf samples are weighed, add in concentrated nitric acid, obtain mixing sample b, the volumetric usage of the concentrated nitric acid is with red bayberry
The quality of leaf subsample is calculated as 18mL/g；
(c) strawberry tree root soil sample is weighed, it is 5 to add in volume ratio：1 chloroazotic acid and the mix acid liquor of hydrofluoric acid, are mixed
Sample c is closed, the volumetric usage of the mix acid liquor is calculated as 40mL/g with the quality of strawberry tree root soil sample；
(B) sample purification：By strontium specific resin wet method dress post, pillar is alternately cleaned 2~3 times with the nitric acid and water of 1+1, Ran Houyi
It is secondary that pillar then with the nitric acid of 3mol/L is balanced with the nitric acid of 1+1,6mol/L hydrochloric acid and washing column, take prepared by step (A) respectively
Digestion solution a, b or c upper prop is first eluted with 3mol/L nitric acid, then elutes strontium with 0.03mol/L nitric acid, collects strontium eluent in poly-
Tetrafluoroethene sample dissolving cup is heated on electric hot plate and is evaporated, and respectively obtains strontium sample a, b, c；
(C) isotopic ratio of strontium is measured using hot surface ionization mass spectrometer：
(C-1) pretreatment of sample band
Rhenium band is first put into immersion 30min~60min in ethyl alcohol, after taking-up is dried, rhenium band is spoted weld on sample introduction stent, then
Degassing in device of air is placed in, the rhenium band pre-processed；
(C-2) the painting sample of strontium
With micropipettor pipette 1 μ L tantalum pentafluoride cast charge be added on pretreatment rhenium band center, energization is evaporated, by step
(B) strontium sample a, b or the c prepared is dissolved respectively with the nitric acid of mass fraction 3%, is then put at the tantalum pentafluoride of rhenium band, is led to
Electricity is evaporated, and 1 μ L tantalum pentafluoride cast charges are added dropwise at sample, and energization is evaporated, energization reddening sample band, then by sample introduction stent
It is packed into the sample disc of hot surface ionization mass spectrometer；
(C-3) the mass spectrum isotopic ratio detection of strontium
Hot surface ionization mass spectrometer vacuumizes, and vacuum degree reaches 3 × 10-7During Pa, rhenium band is heated, is tested, by temperature control
For system at 1500 ± 50 DEG C, detection obtains the isotopic ratio of strontium87Sr/86Sr；
(2) the Strontium Isotopic Ratios identification red bayberry place of production is utilized
According to the method for step (1), the sample of the strawberry tree different parts of different sources is taken to measure the isotopic ratio of strontium respectively,
The isotopic ratio of the strontium of the sample of different sources same area is taken to do correlation distribution map, for identifying the red bayberry in the unknown place of production
Set the place of production situation of sample.
2. the method as described in claim 1, it is characterised in that in the step (A), the red bayberry sample, red bayberry leaf sample
Product or strawberry tree root soil sample are after respectively drying red bayberry, red bayberry leaf or strawberry tree root soil, to be cut with ceramics
Knife is cut small, then is ground with mortar obtained.
3. the method as described in claim 1, it is characterised in that in the step (A), the microwave dissolver uses Anton Paar
The Multiwave3000 microwave dissolvers of company's production.
4. the method as described in claim 1, it is characterised in that in the step (B), the nitric acid of the 1+1 be by concentrated nitric acid and
Water by volume 1：1 mixed preparing obtains.
5. the method as described in claim 1, it is characterised in that in the step (B), the strontium specific resin is SR Resin-
B-tree fat.
6. the method as described in claim 1, it is characterised in that in the step (B), after eluting strontium with 0.03mol/L nitric acid,
Pillar of living again is cleaned according to the following steps：Successively with 6mol/L hydrochloric acid, the nitric acid of 1+1 and washing column.
7. the method as described in claim 1, it is characterised in that the step (B) operates by the following method：
By strontium specific resin wet method dress post, pillar is alternately cleaned 2~3 times with the nitric acid and water of 1+1, then successively with 5 times of cylinders
The washing column of the nitric acid of long-pending 1+1, the 6mol/L hydrochloric acid of 10 times of column volumes and 10 times of column volumes, then the 3mol/ with 5 times of column volumes
The nitric acid balance pillar of L, digestion solution a, b or c upper prop that step (A) is taken to prepare respectively, first with the 3mol/L nitre of 15 times of column volumes
Acid elution, then elute strontium with the 0.03mol/L nitric acid of 12.5 times of column volumes collects strontium eluent in polytetrafluoroethylene (PTFE) sample dissolving cup,
It heats and is evaporated on electric hot plate, respectively obtain strontium sample a, b, c；Again successively with the 6mol/L hydrochloric acid of 10 times of column volumes, 10 times of columns
The water of the nitric acid of the 1+1 of volume and 10 times of column volumes cleans pillar of living again.
8. the method as described in claim 1, it is characterised in that in the step (C-2), the tantalum pentafluoride cast charge press with
Lower ratio is prepared：0.02g tantalic chlorides are weighed in polytetrafluoroethylene (PTFE) sample dissolving cup, 300 μ L water is added in, makes its hydrolysis, after 2h successively
20 μ L hydrofluoric acid, the concentrated phosphoric acid of 20 μ L mass fractions 85%, 200 μ L concentrated nitric acids and 800 μ L water are added in, are closed the lid in electric hot plate
Upper heating makes it dissolve and balance, and the tantalum pentafluoride cast charge is made.
A kind of 9. method for measuring the Strontium Isotopic Ratios in strawberry tree different parts sample, it is characterised in that the method includes
Following steps：
(A) sample pre-treatments：Weigh strawberry tree different parts sample, the strawberry tree different parts sample include red bayberry sample,
Strawberry tree Leaf samples or strawberry tree root soil sample, are then respectively adding digestive reagent, obtain mixing sample a, b or c, point
It is not placed in microwave dissolver and is cleared up, the temperature program for setting microwave dissolver is：5min is raised to 400w, keeps 5min,
5min rises to 800w again, keeps 5min, cooling down to room temperature, the heating of gained mixed liquor is evaporated, after being dissolved with 3mol/L nitric acid
Centrifugation, it is spare to respectively obtain digestion solution a, b or c；
It is described to weigh strawberry tree different parts sample, digestive reagent is separately added into, mixing sample a, b or c are obtained, specifically by following
Operation：
(a) red bayberry sample is weighed, adds in concentrated nitric acid, obtains mixing sample a, the volumetric usage of the concentrated nitric acid is with red bayberry sample
Quality is calculated as 10mL/g；
(b) strawberry tree Leaf samples are weighed, add in concentrated nitric acid, obtain mixing sample b, the volumetric usage of the concentrated nitric acid is with red bayberry
The quality of leaf subsample is calculated as 18mL/g；
(c) strawberry tree root soil sample is weighed, it is 5 to add in volume ratio：1 chloroazotic acid and the mix acid liquor of hydrofluoric acid, are mixed
Sample c is closed, the volumetric usage of the mix acid liquor is calculated as 40mL/g with the quality of strawberry tree root soil sample；
(B) sample purification：By strontium specific resin wet method dress post, pillar is alternately cleaned 2~3 times with the nitric acid and water of 1+1, Ran Houyi
It is secondary that pillar then with the nitric acid of 3mol/L is balanced with the nitric acid of 1+1,6mol/L hydrochloric acid and washing column, take prepared by step (A) respectively
Digestion solution a, b or c upper prop is first eluted with 3mol/L nitric acid, then elutes strontium with 0.03mol/L nitric acid, collects strontium eluent in poly-
Tetrafluoroethene sample dissolving cup is heated on electric hot plate and is evaporated, and respectively obtains strontium sample a, b, c；
(C) isotopic ratio of strontium is measured using hot surface ionization mass spectrometer：
(C-1) pretreatment of sample band
Rhenium band is first put into immersion 30min~60min in ethyl alcohol, after taking-up is dried, rhenium band is spoted weld on sample introduction stent, then
Degassing in device of air is placed in, the rhenium band pre-processed；
(C-2) the painting sample of strontium
With micropipettor pipette 1 μ L tantalum pentafluoride cast charge be added on pretreatment rhenium band center, energization is evaporated, by step
(B) strontium sample a, b or the c prepared is dissolved respectively with the nitric acid of mass fraction 3%, is then put at the tantalum pentafluoride of rhenium band, is led to
Electricity is evaporated, and 1 μ L tantalum pentafluoride cast charges are added dropwise at sample, and energization is evaporated, energization reddening sample band, then by sample introduction stent
It is packed into the sample disc of hot surface ionization mass spectrometer；
(C-3) the mass spectrum isotopic ratio detection of strontium
Hot surface ionization mass spectrometer vacuumizes, and vacuum degree reaches 3 × 10-7During Pa, rhenium band is heated, is tested, by temperature control
For system at 1500 ± 50 DEG C, detection obtains the isotopic ratio of strontium87Sr/86Sr。
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