CN109507274A - A kind of discrimination method of rice geographical sign - Google Patents
A kind of discrimination method of rice geographical sign Download PDFInfo
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- CN109507274A CN109507274A CN201811297661.XA CN201811297661A CN109507274A CN 109507274 A CN109507274 A CN 109507274A CN 201811297661 A CN201811297661 A CN 201811297661A CN 109507274 A CN109507274 A CN 109507274A
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/286—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q involving mechanical work, e.g. chopping, disintegrating, compacting, homogenising
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/40—Concentrating samples
- G01N1/4044—Concentrating samples by chemical techniques; Digestion; Chemical decomposition
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/62—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating the ionisation of gases, e.g. aerosols; by investigating electric discharges, e.g. emission of cathode
- G01N27/626—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating the ionisation of gases, e.g. aerosols; by investigating electric discharges, e.g. emission of cathode using heat to ionise a gas
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/286—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q involving mechanical work, e.g. chopping, disintegrating, compacting, homogenising
- G01N2001/2866—Grinding or homogeneising
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Abstract
The invention discloses a kind of discrimination methods of rice geographical sign, comprising the following steps: tests the pretreatment of rice sample；S2 tests the high-throughput open type electric heating reflux resolution of rice sample；S3 is measured while testing several kinds of mineral elements in rice sample；S4, the rice place of production are traced to the source the building of model；S5, the pretreatment of rice sample to be measured；S6, the high-throughput open type electric heating of rice sample to be measured, which flows back, to be cleared up；S7 is measured while several kinds of mineral elements in rice sample to be measured；S8, date comprision and the rice place of production determine.The present invention is measured the content of 28 kinds of mineral elements in the rice in each place of production, and it establishes rice and traces to the source place of production model, and the test rice sample quantity foot in each place of production, the model that makes to trace to the source is more representative, the accuracy that the place of production is traced to the source is improved, and detection method is simple, it is easy to operate, detection efficiency is high, can promote the use of.
Description
Technical field
The present invention relates to rice geographical sign technical field more particularly to a kind of discrimination methods of rice geographical sign.
Background technique
Geography symbol product, which refers to, originates from specific region, and possessed quality, reputation or other characteristics are essentially dependent on
The natural cause and Humanistic Factors in the place of production, the product being named through audit approval with geographic name.Geography symbol product is opened
Hair and its specialty industries cultivation have become Regional Economic Development new growth point, are growing local economy, the adjustment industrial structure, are increasing
Add farmers' income and expand employment etc. plays an important role.However, China is also for geography symbol product brand protection
There are law sides and technical deficiency.
5 constant virtues rice, Qiqihar rice and build space rice are the geographical sign rice to gain national fame.It is full of in the market
Largely palm off the rice of three kinds of geographical signs, upset market order, compromised the interests of peasant, and the prior art
Under, lack the technology that can effectively identify the rice place of production, so that there are certain difficulties to the protection of certified products rice, we are designed thus
A kind of discrimination method of rice geographical sign is gone out to solve problem above.
Summary of the invention
The purpose of the present invention is to solve disadvantages existing in the prior art, and a kind of rice geographical sign proposed
Discrimination method.
To achieve the goals above, present invention employs following technical solutions:
A kind of discrimination method of rice geographical sign, comprising the following steps:
S1 tests the pretreatment of rice sample: take 1kg test rice sample quartering division to 300g, it then will examination
It tests rice sample and is put into be crushed in agate mortar or the ball mill of agate material and all analyzed by the nylon in 100 mesh apertures
Sieve, is sub-packed in closed preservation in polyethylene can；
S2 tests the high-throughput open type electric heating reflux resolution of rice sample: after the crushing for accurately weighing 0.2g in S1
Rice sample is tested, is placed in 100mL high-boron-silicon glass digestion tube, 10mL two end number mixing digestion agent is added, shakes up, covers funnel
At least 2h is stood at room temperature, is placed on electric heating resolution instrument, is warming up to 115 DEG C (mercury is warming up to 75 DEG C), 1.5h is kept, after of continuing rising
Temperature keeps 3.5h to 155 DEG C (mercury is warming up to 115 DEG C), and taking-up is cooled to room temperature, and digestion solution is transferred to 25mL Glass capacity bottle
In, inside pipe wall is cleared up with 3 flushings of a small amount of moisture, merges washing lotion into volumetric flask, is settled to scale with water, takes supernatant after standing
Machine measures on liquid 10mL；
S3 is measured while testing several kinds of mineral elements in rice sample: digestion solution in S2 using highly sensitive and
High jamproof icp ms (ICP-MS) carry out while measuring, and obtain beryllium (Be), sodium (Na), magnesium
(Mg), aluminium (Al), phosphorus (P), potassium (K), calcium (Ca), vanadium (V), chromium (Cr), manganese (Mn), iron (Fe), cobalt (Co), nickel (Ni), copper
(Cu), zinc (Zn), arsenic (As), selenium (Se), rubidium (Rb), strontium (Sr), molybdenum (Mo), silver (Ag), cadmium (Cd), antimony (Sb), barium (Ba), mercury
(Hg), totally 28 kinds of elements are testing the content in rice sample respectively for thallium (Tl), lead (Pb), uranium (U)；
S4, the rice place of production are traced to the source the building of model: homemade Data Analysis Software are utilized, to the test rice sample of measurement
In 28 kinds of constituent contents carry out multiple regression analysis, the rice place of production for constructing group test rice sample several kinds of mineral elements is traced to the source
Model；
S5, the pretreatment of rice sample to be measured: using the preprocess method of S1 test rice sample, to rice sample to be measured
It is pre-processed and is saved；
S6, the high-throughput open type electric heating of rice sample to be measured, which flows back, to be cleared up: using the method in S2, to rice sample to be measured
Product are cleared up；
S7 is measured in rice sample to be measured while several kinds of mineral elements: using the method in S3, to rice sample to be measured
28 kinds of constituent contents in digestion solution are measured；
S8, date comprision and the rice place of production determine: 28 kinds of mineral elements in the rice sample to be measured measured are contained
Amount is input to rice constructed by S4 and traces to the source in model, according to software calculated result, determines whether the rice sample is that test is big
Rice sample comes from the same place of production.
Preferably, the two end number mixing digestion agent for the nitric acid and hydrogen peroxide that ratio is 8.5: 1.5 has been used in the S2 and S6.
Preferably, in the S1 and S5 when the processing of test rice sample and rice sample to be measured, grinding device and sample
The material of contact portion is agate, and analysis sieve material is nylon material, and storage container is polyethylene material.
Preferably, for the S3 detection elements when testing the content in rice sample, to use yttrium (Y) is internal standard, and big
Rice Specimen eliminating liquid while sample introduction, the drift to the signal that rectifies an instrument.
Preferably, blank and rice substrate standard substance are measured in the treatment process of the S2 simultaneously, as Quality Control side
Formula, blank value will be lower than method detection limit, and substrate standard substance each element measured value will be in defined error range.
Preferably, in the S4, before Database, the quantity of the test rice sample in each place of production is at least 50 parts.
Compared with prior art, the beneficial effects of the present invention are:
1, when the processing of test rice sample and rice sample to be measured, the material of grinding device and sample contact portion is Ma
Nao, analysis sieve material is nylon material, and storage container is polyethylene material, effectively prevents experimental facilities and vessel to sample
Pollution, sample comminution granularity are 100 mesh, are greatly improved resolution efficiency；
2, in the high-throughput open type electric heating reflux resolution operation for carrying out rice sample, the step that high temperature catches up with acid is avoided
Suddenly, a possibility that significantly reducing first procatarxis high temperature and losing, make to operate it is simpler effectively, and improve detection effect
Rate；
3, it when element determination, has used sensitivity higher and the stronger ICP-MS technology of anti-interference ability, has improved sensitivity
While with anti-interference ability, measurement while realizing multielement greatly improves detection efficiency；
4, the content of 28 kinds of mineral elements in the rice in each place of production is measured, and establishes rice and traces to the source place of production mould
Type, and the test rice sample quantity foot in each place of production, the model that makes to trace to the source is more representative, improve the place of production trace to the source it is accurate
Property；
5, detection method is simple, easy to operate, can promote the use of.
Detailed description of the invention
Fig. 1 is a kind of flow chart of the discrimination method of rice geographical sign proposed by the present invention.
Specific embodiment
The technical scheme in the embodiments of the invention will be clearly and completely described below, it is clear that described implementation
Example is only a part of the embodiment of the present invention, instead of all the embodiments.
A kind of discrimination method of rice geographical sign, comprising the following steps:
S1 tests the pretreatment of rice sample: take 1kg test rice sample quartering division to 300g, it then will examination
It tests rice sample and is put into be crushed in agate mortar or the ball mill of agate material and all analyzed by the nylon in 100 mesh apertures
Sieve, is sub-packed in closed preservation in polyethylene can；
S2 tests the high-throughput open type electric heating reflux resolution of rice sample: after the crushing for accurately weighing 0.2g in S1
Rice sample is tested, is placed in 100mL high-boron-silicon glass digestion tube, 10mL two end number mixing digestion agent is added, shakes up, covers funnel
At least 2h is stood at room temperature, is placed on electric heating resolution instrument, is warming up to 115 DEG C (mercury is warming up to 75 DEG C), 1.5h is kept, after of continuing rising
Temperature keeps 3.5h to 155 DEG C (mercury is warming up to 115 DEG C), and taking-up is cooled to room temperature, and digestion solution is transferred to 25mL Glass capacity bottle
In, inside pipe wall is cleared up with 3 flushings of a small amount of moisture, merges washing lotion into volumetric flask, is settled to scale with water, takes supernatant after standing
Machine measures on liquid 10mL；
S3 is measured while testing several kinds of mineral elements in rice sample: digestion solution in S2 using highly sensitive and
High jamproof icp ms (ICP-MS) carry out while measuring, and obtain beryllium (Be), sodium (Na), magnesium
(Mg), aluminium (Al), phosphorus (P), potassium (K), calcium (Ca), vanadium (V), chromium (Cr), manganese (Mn), iron (Fe), cobalt (Co), nickel (Ni), copper
(Cu), zinc (Zn), arsenic (As), selenium (Se), rubidium (Rb), strontium (Sr), molybdenum (Mo), silver (Ag), cadmium (Cd), antimony (Sb), barium (Ba), mercury
(Hg), totally 28 kinds of elements are testing the content in rice sample respectively for thallium (Tl), lead (Pb), uranium (U), and it be interior for using yttrium (Y)
Mark, and rice sample digestion solution sample introduction simultaneously, the drift to the signal that rectifies an instrument；
S4, the rice place of production are traced to the source the building of model: homemade Data Analysis Software are utilized, to the test rice sample of measurement
In 28 kinds of constituent contents carry out multiple regression analysis, the rice place of production for constructing group test rice sample several kinds of mineral elements is traced to the source
Model, and the quantity for testing rice sample is at least 50 parts；
S5, the pretreatment of rice sample to be measured: using the preprocess method of S1 test rice sample, to rice sample to be measured
It is pre-processed and is saved；
S6, the high-throughput open type electric heating of rice sample to be measured, which flows back, to be cleared up: using the method in S2, to rice sample to be measured
Product are cleared up；
S7 is measured in rice sample to be measured while several kinds of mineral elements: using the method in S3, to rice sample to be measured
28 kinds of constituent contents in digestion solution are measured；
S8, date comprision and the rice place of production determine: 28 kinds of mineral elements in the rice sample to be measured measured are contained
Amount is input to rice constructed by S4 and traces to the source in model, according to software calculated result, determines whether the rice sample is that test is big
Rice sample comes from the same place of production.
The foregoing is only a preferred embodiment of the present invention, but scope of protection of the present invention is not limited thereto,
Anyone skilled in the art in the technical scope disclosed by the present invention, according to the technique and scheme of the present invention and its
Inventive concept is subject to equivalent substitution or change, should be covered by the protection scope of the present invention.
Claims (6)
1. a kind of discrimination method of rice geographical sign, which comprises the following steps:
S1 tests the pretreatment of rice sample: taking 1kg test rice sample quartering division to 300g, then will test big
Rice sample, which is put into, is crushed to all nylon analysis sieves by 100 mesh apertures in agate mortar or the ball mill of agate material, point
Loaded on preservation closed in polyethylene can；
S2 tests the high-throughput open type electric heating reflux resolution of rice sample: testing after the crushing for accurately weighing 0.2g in S1
Rice sample is placed in 100mL high-boron-silicon glass digestion tube, and 10mL two end number mixing digestion agent is added, shakes up, covers funnel in room
Temperature is lower to stand at least 2h, is placed on electric heating resolution instrument, is warming up to 115 DEG C (mercury is warming up to 75 DEG C), keeps 1.5h, be continuously heating to
155 DEG C (mercury is warming up to 115 DEG C), 3.5h is kept, taking-up is cooled to room temperature, digestion solution is transferred in 25mL Glass capacity bottle,
Inside pipe wall is cleared up with 3 flushings of a small amount of moisture, merges washing lotion into volumetric flask, is settled to scale with water, takes supernatant after standing
The upper machine measurement of 10mL；
S3 is measured while testing several kinds of mineral elements in rice sample: the digestion solution in S2 uses highly sensitive and highly resistance
The icp ms (ICP-MS) of interference are carried out while being measured, and obtain beryllium (Be), sodium (Na), magnesium (Mg), aluminium
(Al), phosphorus (P), potassium (K), calcium (Ca), vanadium (V), chromium (Cr), manganese (Mn), iron (Fe), cobalt (Co), nickel (Ni), copper (Cu), zinc
(Zn), arsenic (As), selenium (Se), rubidium (Rb), strontium (Sr), molybdenum (Mo), silver (Ag), cadmium (Cd), antimony (Sb), barium (Ba), mercury (Hg), thallium
(Tl), totally 28 kinds of elements are testing the content in rice sample respectively for lead (Pb), uranium (U)；
S4, the rice place of production are traced to the source the building of model: homemade Data Analysis Software are utilized, in the test rice sample of measurement 28
Kind of constituent content carries out multiple regression analysis, and the rice place of production for constructing group test rice sample several kinds of mineral elements is traced to the source mould
Type；
The pretreatment of rice sample to be measured: S5 using the preprocess method of S1 test rice sample, carries out rice sample to be measured
Pretreatment and preservation；
S6, the high-throughput open type electric heating of rice sample to be measured flow back resolution: using the method in S2, to rice sample to be measured into
Row resolution；
S7 is measured while several kinds of mineral elements in rice sample to be measured: using the method in S3, being cleared up to rice sample to be measured
28 kinds of constituent contents in liquid are measured；
S8, date comprision and the rice place of production determine: the content of 28 kinds of mineral elements in the rice sample to be measured measured is defeated
Enter to rice constructed by S4 and trace to the source in model, according to software calculated result, determines whether the rice sample is test rice sample
Product come from the same place of production.
2. a kind of discrimination method of rice geographical sign according to claim 1, which is characterized in that make in the S2 and S6
With the two end number mixing digestion agent of nitric acid and hydrogen peroxide that ratio is 8.5: 1.5.
3. a kind of discrimination method of rice geographical sign according to claim 1, which is characterized in that S1 the and S5 pilot scale
When testing the processing of rice sample and rice sample to be measured, the material of grinding device and sample contact portion is agate, analysis sieve material
Matter is nylon material, and storage container is polyethylene material.
4. a kind of discrimination method of rice geographical sign according to claim 1, which is characterized in that the S3 detection elements
When testing the content in rice sample, to use yttrium (Y) is internal standard, and rice sample digestion solution sample introduction simultaneously, to correct
The drift of instrument signal.
5. a kind of discrimination method of rice geographical sign according to claim 1, which is characterized in that the S2's is processed
Blank and rice substrate standard substance are measured in journey simultaneously, as Quality Control mode, blank value will be lower than method detection limit, matrix
Standard substance each element measured value will be in defined error range.
6. a kind of discrimination method of rice geographical sign according to claim 1, which is characterized in that in the S4, data
Before library is established, the quantity of the test rice sample in each place of production is at least 50 parts.
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| CN201811297661.XA CN109507274A (en) | 2018-10-23 | 2018-10-23 | A kind of discrimination method of rice geographical sign |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN117990772A (en) * | 2024-04-07 | 2024-05-07 | 中国科学院生态环境研究中心 | Method for determining phosphorus element in plant by utilizing ICP-MS |
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| CN102564834A (en) * | 2011-12-19 | 2012-07-11 | 攀钢集团攀枝花钢铁研究院有限公司 | Digestion method of metallurgical materials and detection method |
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Application publication date: 20190322 |