CN108663468A - A kind of preparation method of wheat flour Analysis on amino acid components standard substance - Google Patents
A kind of preparation method of wheat flour Analysis on amino acid components standard substance Download PDFInfo
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- CN108663468A CN108663468A CN201810645111.6A CN201810645111A CN108663468A CN 108663468 A CN108663468 A CN 108663468A CN 201810645111 A CN201810645111 A CN 201810645111A CN 108663468 A CN108663468 A CN 108663468A
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N2030/042—Standards
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Abstract
The invention discloses a kind of preparation methods of wheat flour Analysis on amino acid components standard substance.The wheat flour without any additive is chosen first, the wheat flour of selection is sieved with 100 mesh sieve into carry out screening and removing impurities, and soak degreasing in solvent is added in wheat flour after removal of impurities；Wheat flour after degreasing is spontaneously dried and is dried successively, and wheat flour sample is obtained, and sample carries out irradiation inactivated after packing, is finally vacuum-packed, is preserved under the conditions of 20 DEG C after packaging.Wheat flour Analysis on amino acid components standard substance has been prepared using the present invention, solves critical issue existing in the prior art, the domestic blank that there is no wheat flour powder sample amino acid standard matter is filled up, the Development Level to improve China's health of masses, food, environment etc. standard substance is laid a good foundation.
Description
One, technical field：
The present invention relates to a kind of preparation methods of standard substance, more particularly to a kind of wheat flour Analysis on amino acid components
The preparation method of standard substance.
Two, technical background：
14% or so, uniformity, the protein level of very close mixed feed passes through protein content in wheat flour
After processing can long-term preservation, be suitble to do the amino acid standard matter of low protein level.Currently, amino acid analysis method is mainly adopted
With the national standard method GB/T 18246 and column front derivation reversed-phased high performace liquid chromatographic of automatic amino acid analyzer.According to
National standard is accordingly detected, and corresponding forage standard substance is needed.Currently, there is amino acid mixed solution reference substance in China
Matter (number：GBW (E) 100062), but the Analysis on amino acid components standard substance using wheat flour as matrix is still blank.
Substrate standard substance is measuring process control, the important carrier that method confirms, arbitration and examination verification are evaluated, and is
Ensure that measurement result is reliable, promotes the important support of laboratory testing capability.When detecting feed matrix sample, matrix effect is past
Toward being one of systematic error source, influence result it is accurate whether.The actually detected sample of user should be selected to match as far as possible
Substrate standard substance reduces the operating cost in laboratory, improves the validity and reliability of testing result.Amino in wheat flour
The development of sour component analytical standard substance, acts not only as a kind of etalon, come determine in wheat flour sample amino acid at
Divide content；Meanwhile it can also be used as a kind of standard sample, it is whether reasonable come the method that detects sample pre-treatments.This is for small
The pre-treating method of flour also plays the effect of a supervision and inspection so that the safety verification of wheat flour is more reasonable and tight
Sincerely.Currently, the pre-treatment and analysis valued methods research of wheat flour are always the key of research, so there is an urgent need to develop
A kind of wheat flour matrix amino acid standard matter.
Three, invention content：
The technical problem to be solved by the present invention is to：In order to solve to there is no wheat flour matrix amino acid standard matter at present
Defect, the present invention provide a kind of preparation method of wheat flour Analysis on amino acid components standard substance.
To solve the above-mentioned problems, the technical solution adopted by the present invention is that：
The present invention provides a kind of preparation method of wheat flour Analysis on amino acid components standard substance, the preparation method packet
Include following steps：
A, it selects：Choose the flour without any additive；
B, impurity elimination：The flour of selection is sieved with 100 mesh sieve into carry out screening and removing impurities；
C, degreasing：It will be impregnated in wheat flour complete wetting to solvent after step b impurity eliminations, every 2 in soaking process~
It is sufficiently stirred within 4 hours once, soaking time is 12~15 hours, is filtered after immersion, and solvent is filtered, and it is same to replace novel solvent
Sample impregnates once again, and the wheat flour of degreasing is obtained after immersion treatment；
D, drying：The wheat flour obtained after step c degreasings is naturally shady and cool 4~6 hours dry, it is put into after natural drying
It is dried in vacuum drying chamber, obtains wheat flour sample after drying, moisture ＜ 1% in wheat flour sample；
E, it dispenses：Wheat flour sample after step d dryings is sub-packed in vial, and covers tightly threaded cap, seals sample
Specification is 5g/ bottles；
F, irradiation inactivated：The sample of packing is used60Co gamma-ray irradiations inactivate, and dose intensity is 7kGy~10kGy,
The irradiation inactivated time is 2 hours；
G, the sample after step f irradiation inactivateds is vacuum-packed using aluminum foil compound bag, after packaging under the conditions of -20 DEG C
It preserves.
According to the preparation method of above-mentioned wheat flour Analysis on amino acid components standard substance, solvent described in step c is nothing
Any one of water ether, petroleum ether, acetone, n-hexane, methanol and ethyl alcohol.
According to the preparation method of above-mentioned wheat flour Analysis on amino acid components standard substance, the solvent be petroleum ether or
Anhydrous ether.
According to the preparation method of above-mentioned wheat flour Analysis on amino acid components standard substance, spontaneously dried described in step d
It is that the wheat flour tiling after degreasing is placed in enamel basin to be dried under the conditions of natural environment non-direct sunlight.
According to the preparation method of above-mentioned wheat flour Analysis on amino acid components standard substance, vacuum is put into described in step d
It is carried out in drying course in drying box, drying temperature is 80~105 DEG C, and drying time is 3~6 hours.
According to the preparation method of above-mentioned wheat flour Analysis on amino acid components standard substance, vial is described in step e
The brown bottle of threaded mouth.
According to the preparation method of above-mentioned wheat flour Analysis on amino acid components standard substance, step f middle dosage intensity is
7kGy。
The positive beneficial effect of the present invention：
1, the wheat flour substrate standard substance prepared using technical solution of the present invention can ensure closer to actual sample
The better magnitude tracing of amino acid detection project in wheat flour, it is as a result relatively reliable and comparable, caused by solving matrix difference
Testing result difference problem improves magnitude tracing level, foundation is provided for the judgement of wheat albinism line.
2, the wheat flour substrate standard substance prepared using technical solution of the present invention is easy to get, is at low cost.System of the present invention
Standby standard substance stability is good, can under the conditions of -20 DEG C long-term preservation (at least a year), there is preferable uniformity and steady
It is qualitative.
3, wheat flour Analysis on amino acid components standard substance prepared by the present invention, solves pass existing in the prior art
Key problem has filled up the domestic blank that there is no wheat flour amino acid standard matter, to improve China's health of masses, food, environment
Etc. the Development Level of standard substance lay a good foundation.
4, the present invention has chosen wheat flour as matrix, and the substrate standard substance protein is very close to mixed feed
Protein level, after processing can long-term preservation, be suitble to do the amino acid standard matter of low protein level.
5, the development of wheat flour Analysis on amino acid components standard substance of the present invention, control, product in enterprise product quality
Formulation, the examination and test of products and the quality control of certification authority and evaluation of standard, Laboratory Accreditation aspect suffer from important meaning
Justice, the sound development of the development of the standard substance to China's feed industry improve Animal product quality and play positive promotion and make
With.
Four, it illustrates：
17 kinds of amino acid mixed solution standard substance chromatograms after Fig. 1 derivatization reactions；
Fig. 2 derivative reagent blank chromatograms；
The chromatogram of wheat flour Analysis on amino acid components standard substance sample of the present invention after Fig. 3 derivatization reactions.
Five, specific implementation mode：
The present invention is further explained with reference to embodiments, but is not intended to limit the range of technical solution of the present invention protection.
Embodiment 1：
The preparation method of wheat flour Analysis on amino acid components standard substance of the present invention, the detailed step of the preparation method is such as
Under：
A, it selects：Choose the commercially available wheat flour without any additive；
B, impurity elimination：Wheat flour is first sieved with 100 mesh sieve into carry out screening and removing impurities；
C, degreasing：It will impregnate, impregnated in wheat flour complete wetting to solvent anhydrous ether after step b impurity eliminations
It is sufficiently stirred within every 3 hours in journey once, soaking time is 12 hours, is filtered after immersion, and solvent is filtered, and replaces novel solvent
Anhydrous ether equally impregnates once again, and the wheat flour of degreasing is obtained after immersion treatment；
D, drying：By the wheat flour obtained after step c degreasings, naturally 4 hours shady and cool dry (natural drying is：By degreasing
Wheat flour tiling afterwards is placed in enamel basin to be dried under the conditions of natural environment non-direct sunlight), it is put into after natural drying
It is dried in vacuum drying chamber, drying temperature is 80 DEG C, and drying time is (to be placed in wheat flour tiling when drying and ward off for 3 hours
In ceramic bowl, it is placed into vacuum drying chamber and is dried), obtain wheat flour sample after drying, moisture ＜ in wheat flour sample
1%；
E, it dispenses：Wheat flour sample after step d dryings is sub-packed in the vial of threaded mouth, and covers tightly screw thread
Lid, sealing sample specification is 5g/ bottles, is divided into and fills 500 bottles；
F, irradiation inactivated：The sample of packing is used60Co gamma-ray irradiations inactivate, dose intensity 7kGy, irradiation inactivated
Time is 2 hours；
G, the sample after step f irradiation inactivateds is vacuum-packed using aluminum foil compound bag, after packaging under the conditions of -20 DEG C
It preserves.
It is the dependence test that gained wheat flour Analysis on amino acid components standard substance sample is prepared to embodiment 1 below：
(1) related test results of each processing stage wheat flour sample
Raw material Commercial wheat powder that the present invention uses and by dry (moisture in gained wheat flour sample after dry
＜ 1%) afterwards the Related Component testing result of wheat flour sample refer to table 1.
1 raw material Commercial wheat powder of table and after drying wheat flour sample Related Component testing result
| Protein (%) | Fatty (%) | Moisture (%) | |
| Commercial wheat powder | 12.4 | 0.1 | 13.4 |
| Wheat flour sample after drying | 13.8 | 0.8 | 0.9 |
During the preparation method of wheat flour Analysis on amino acid components standard substance of the present invention, the gained sample after packing
Testing result of the product before and after irradiation inactivated refers to table 2 and table 3.
The testing result of gained sample before irradiation inactivated after packing of table 2
| Title | Total number of bacteria (a/g) | Total number of molds (a/g) |
| Wheat flour | 3300000 | <10 |
The testing result of gained sample after irradiation inactivated after packing of table 3
It indicates：From the above data, it uses60The dose intensity of Co γ be 7kGy x ray irradiation xs inactivate 2 hours be best spoke
According to dosage.
(2) present invention prepares inspection and the definite value of gained wheat flour Analysis on amino acid components standard substance sample
The present invention carries out analysis measurement using pre-column derivatization-ultra-performance liquid chromatography, and specific determination condition is such as
Under：
Instrument：Ultra performance liquid chromatography matches ultraviolet-visible detector (Waters, the U.S.)；
Liquid phase chromatogram condition：
Chromatographic column：AccQ-TAGTM ULTRA C18(2.1 × 100mm, 1.7 μm)；
Mobile phase：A：AccQTag eluents A (10 times of dilution), B：AccQTag eluents B；
Flow velocity：0.7mL/min；
Column temperature：55℃；
Ultraviolet detection wavelength：260nm；
Sample size：1μL；
According to the gradient that mobile phase is arranged in table 4, separate run times 9.5min.
The liquid phase gradient table of 4 derivatization method of table
Wheat flour Analysis on amino acid components standard substance prepared by the present invention uses pre-column derivatization-ultra high efficiency liquid phase color
The processing procedure that spectrometry is analyzed is as follows：
1) pre-treatment of Analysis on amino acid components standard substance：
Sour water solution：The wheat flour Analysis on amino acid components standard substance for weighing the preparation of the 0.3g embodiment of the present invention 1 is added to
10mL, a concentration of 6mol/L hydrochloric acid solution in, then hydrolyzed 22 hours under the conditions of 110 DEG C；50mL appearances are filled into after hydrolysis
In measuring bottle, with water constant volume, the hydrolyzation sample of wheat flour Analysis on amino acid components standard substance is made.
2) preparation of AccQ-Fluor derivative reagents：
AccQ-Fluor derivating agent powder is diluted first, the acetonitrile that 1mL is drawn using pipettor is added to derivative
It is sealed in reagent bottle, the addition of agent powder derived from reagent bottle is 1mg, vortex mixed 15 seconds；Then it is being preheating to
Heating in 55 DEG C of baking oven, to dissolve all derivative reagent powder, heating time is 8 minutes, the AccQ- prepared
Fluor derivative reagents.
3) wheat flour Analysis on amino acid components reference substance prepared by 17 kinds of amino acid mixed solution standard substances and the present invention
The derivatization reaction of quality sample：
The derivatization reaction of 17 kinds of amino acid mixed solution standard substances (by amino acid converting for stable AQC derivatives)：
Baking oven is opened and constant temperature is to 55 DEG C, 10 μ L, 17 kinds of amino acid mixed solution standard substances is taken to inject clean derivative tube bottom
Then portion is added in 70 μ L AccQ-Fluor Buffer1 borate buffers to derivative pipe, vortex mixed finally draws 20 μ L
The derivative reagent of above-mentioned preparation is added under vorticity in derivative pipe, and keeps vortex mixed 15 seconds, after vortex mixed
Gained derivative products are transferred in derivative dedicated micro-sampling bottle, and it is molten to obtain the mixing of 17 kinds of amino acid after derivatization reaction
Liquid standard substance.
The derivatization reaction of wheat flour Analysis on amino acid components standard substance sample prepared by the present invention：With above-mentioned 17 kinds of ammonia
The derivatization reaction of base acid mixed solution standard substance.
The derivative reagent used is purchased from the AccQ-Fluor reagent packets of Waters companies production.
By 17 kinds of amino acid mixed solution standard substances, the wheat flour aminoacid ingredient of the present invention after above-mentioned derivatization reaction
Analytical standard material sample, which is placed in 55 DEG C of thermostatic drying chambers, heats 10min, then cools to room temperature, to be measured.According to above-mentioned
The determination condition of pre-column derivatization-ultra-performance liquid chromatography of restriction is to 17 kinds of amino acid mixed solutions after derivatization reaction
Wheat flour Analysis on amino acid components standard substance sample of the present invention difference after standard substance, derivative reagent blank, derivatization reaction
It is detected, obtained chromatogram refers to attached drawing 1-3.
The chromatogram of 17 kinds of amino acid mixed solution standard substances after derived from attached drawing 1 has inside including reagent peak
18 chromatographic peaks, are followed successively by according to the sequencing of retention time：His, Ser, Arg, Gly, Asp, Glu, Thr, Ala, Pro,
Deriv (derivative reagent peak), Cys, Lyr, Tyr, Met, Val, Ile, Leu, Phe.
It is small by the present invention after control 17 kinds of amino acid mixed solution standard substances, derivative reagent blank, derivatization reactions
The chromatogram of flour Analysis on amino acid components standard substance sample, it may be determined that the wheat flour standard substance prepared by the present invention
The type and its content of middle amino acid.
(4) uniformity to the wheat flour Analysis on amino acid components standard substance prepared by the present invention, study on the stability,
And the analysis of definite value and uncertainty：
1) uniformity testing：
According to the requirement of national standard reference material technology specification (JJG 1006-1994), carried out using variance analysis
Uniformity test.25 samples are extracted from wheat flour Analysis on amino acid components standard substance sample prepared by the present invention to be used for
Uniformity testing, each sample measure 3 progress variance analyses, are judged by the comparison of between-group variance and intra-class variance each
Whether there is or not system deviations between group measured value.
By the above uniformity testing, gained inventive samples uniformity testing is the results detailed in Table 5.
The Evaluation for Uniformity result of wheat flour Analysis on amino acid components standard substance prepared by 5 present invention of table
The wheat flour Analysis on amino acid components standard substance sample prepared according to the detection evaluation result judgement present invention is equal
Even.
2) study on the stability：
It is by multiple samples (a collection of sample) that are of the invention while preparing, under the same conditions that long-time stability, which are investigated,
It is measured with the continuity of time.In 24 months, to the wheat flour Analysis on amino acid components standard substance of the invention prepared
7 study on the stability are carried out, respectively on the day of sample preparation, after 1 month, after 2 months, after 3 months, after 6 months, 12
3 are randomly selected after month and to the standard substance of preparation after 24 months, every is surveyed 3 times, is positioned at -20 DEG C and 4 DEG C and is preserved,
Carry out long-time stability investigation.
Line fitting approach is selected to evaluate its stability.The time is represented with X, the characteristic of standard substance is represented with Y
Value, fitting is in alignment, then has slope β1
Intercept is calculated by following formula：
The standard deviation of straight line can be calculated by following formula：
When | β1| ＜ t0.95,n-2·s(β1) when slope be inapparent, be judged to not observe unstability.
Short-term stability, which is investigated, uses synchronism stability Journal of Sex Research, is introduced into so that the measurement in all stability studies exists
Repeatability occurs, i.e., only carries out a wheel calibration.In wheat flour of the present invention Analysis on amino acid components standard substance transportational process,
Stability under the conditions of laboratory temperature in use etc., respectively by standard substance -20 DEG C, 4 DEG C, room temperature, 40 DEG C place 1 day, 2
It, 4 days, 7 days, 15 days and 30 days, the content of amino acid in monitoring standard substance carries out estimation of stability to result.
It is investigated by the above long-time stability, gained long-time stability are investigated the results detailed in Table 6 and table 7.
The long-time stability evaluation result (4 DEG C) of 6 wheat flour Analysis on amino acid components standard substance of the present invention of table
The long-time stability evaluation result (- 20 DEG C) of 7 wheat flour Analysis on amino acid components standard substance of the present invention of table
Long-time stability investigate result：Analysis result shows that standard substance of the present invention is good in 2 year internal stabilities.
It is investigated by the above short-term stability, gained short-term stability is investigated the results detailed in Table 8 and table 9.
Study on the stability result (the room temperature of 8 wheat flour Analysis on amino acid components standard substance of the present invention of table：20±5℃)
The study on the stability result (40 DEG C) of 9 wheat flour Analysis on amino acid components standard substance of the present invention of table
Short-term stability investigates result：The above analysis result shows standard substance of the present invention under traffic condition in 30 days
It is stable, meets actual shipment requirement.
4) definite value of standard substance：
According to ISO directive/guides 35《The rule and statistical method of standard substance/standard sample definite value》It is required that the present invention
The valued methods of the wheat flour Analysis on amino acid components standard substance of preparation use multiple laboratory cooperation valued methods.It invites
Henan Hai Ruizheng detection techniques Co., Ltd, agricultural product quality supervision and inspection center of the Ministry of Agriculture, Henan Province's feed product
Quality monitoring testing station (save veterinary drug and supervise institute), Henan are herded produces through food and feed detection Co., Ltd, Henan Province's grain and oil feed
The common definite value of quality Supervision Test Center.
The organization for participating in cooperation definite value, the analytical instrument used and detection foundation are respectively：
10 definite value laboratory summary sheet of table
The unit of every participation cooperation definite value all randomly selects wheat flour Analysis on amino acid components mark prepared by the present invention
Quasi- substance 11, wherein one is used as practice sample, other 10 samples to carry out pre-treatments, each treated, and increment repeats
It measures 2 times.The pre-treatment of sample is all made of the sour processing method in national standard method GB/T 18246-2000.The survey of sample
Amount method is all made of national standard method GB/T 18246-2000, and each laboratory is due to instrument model difference, specific measurement method
It is operated by instrument specification.
According to above-mentioned experiment, gained definite value is the results detailed in Table 11.
Each laboratory of 11 wheat flour Analysis on amino acid components standard substance of the present invention of table value data that is averaged summarizes
| Amino acid | Laboratory 1 | Laboratory 2 | Laboratory 3 | Laboratory 4 | Laboratory 5 | Laboratory 6 | Asserting value |
| Asparatate | 0.524 | 0.520 | 0.536 | 0.520 | 0.529 | 0.539 | 0.53 |
| Threonine | 0.330 | 0.319 | 0.322 | 0.324 | 0.328 | 0.320 | 0.32 |
| Serine | 0.547 | 0.556 | 0.583 | 0.552 | 0.532 | 0.547 | 0.55 |
| Glutamic acid | 4.503 | 4.569 | 4.577 | 4.412 | 4.497 | 4.588 | 4.52 |
| Glycine | 0.458 | 0.450 | 0.466 | 0.458 | 0.450 | 0.463 | 0.46 |
| Alanine | 0.377 | 0.360 | 0.360 | 0.373 | 0.370 | 0.387 | 0.37 |
| Cystine | 0.136 | 0.142 | 0.149 | 0.143 | 0.138 | 0.145 | 0.14 |
| Valine | 0.551 | 0.548 | 0.537 | 0.551 | 0.538 | 0.544 | 0.54 |
| Methionine | 0.156 | 0.177 | 0.212 | 0.183 | 0.163 | 0.132 | 0.17 |
| Isoleucine | 0.446 | 0.469 | 0.479 | 0.473 | 0.458 | 0.450 | 0.46 |
| Leucine | 0.847 | 0.851 | 0.891 | 0.857 | 0.837 | 0.842 | 0.85 |
| Tyrosine | 0.263 | 0.233 | 0.242 | 0.200 | 0.225 | 0.286 | 0.24 |
| Phenylalanine | 0.655 | 0.661 | 0.649 | 0.651 | 0.638 | 0.614 | 0.64 |
| Lysine | 0.261 | 0.284 | 0.286 | 0.277 | 0.260 | 0.255 | 0.27 |
| Histidine | 0.339 | 0.296 | 0.285 | 0.306 | 0.311 | 0.277 | 0.30 |
| Arginine | 0.459 | 0.480 | 0.492 | 0.443 | 0.452 | 0.463 | 0.46 |
| Proline | 1.361 | 1.479 | 1.430 | 1.498 | 1.433 | 1.409 | 1.44 |
Cooperation definite value conclusion：The result that unit by participating in cooperation definite value is provided meets the requirements, this project
Definite value is finally the average value that cooperation definite value laboratory provides result, as shown in table 11.
5) analysis on Uncertainty：
The uncertainty source of wheat flour Analysis on amino acid components standard substance prepared by the present invention is made of six parts：
The uncertainty of uncertainty, balance weighing introducing that amino acid mixed solution standard substance introduces, peak area ratio measurement introducing
Uncertainty, value data statistics introduce uncertainty, uniformity difference introduce uncertainty and stability introduce
Uncertainty.Analysis on Uncertainty is the results detailed in Table 12 and table 13.
The uncertainty result of 12 wheat flour Analysis on amino acid components standard substance of the present invention of table
The combined standard uncertainty of wheat flour Analysis on amino acid components standard substance of the present invention is multiplied by Coverage factor k=2
Be expanded uncertainty.Gained expanded uncertainty is the results detailed in Table 13.
The extension of 13 wheat flour Analysis on amino acid components standard substance of the present invention of table does not know result
Definite value conclusion：The standard value and uncertainty that the substrate standard substance of the present invention finally determines are as shown in table 13.
Wheat flour Analysis on amino acid components standard substance prepared by the present invention can be that feed factory, testing agency etc. provide
The standard substance consistent with sample to be tested matrix is determined amino acid laboratory to improve the accuracy of determined amino acid
Internal quality control provides reference material；Definite value for feed factory quality-control product provides reference material.
Embodiment 2：
The preparation method of wheat flour Analysis on amino acid components standard substance of the present invention, the detailed step of the preparation method is such as
Under：
A, it selects：Choose the commercially available wheat flour without any additive；
B, impurity elimination：Wheat flour is first sieved with 100 mesh sieve into carry out screening and removing impurities；
C, degreasing：It will impregnate, impregnated in wheat flour complete wetting to solvent anhydrous ether after step b impurity eliminations
It is sufficiently stirred within every 2 hours in journey once, soaking time is 12 hours, is filtered after immersion, and solvent is filtered, and replaces novel solvent
Anhydrous ether equally impregnates once again, and the wheat flour of degreasing is obtained after immersion treatment；
D, drying：By the wheat flour obtained after step c degreasings, naturally 6 hours shady and cool dry (natural drying is：By degreasing
Wheat flour tiling afterwards is placed in enamel basin to be dried under the conditions of natural environment non-direct sunlight), it is put into after natural drying
It is dried in vacuum drying chamber, drying temperature is 105 DEG C, and drying time is (to be placed in wheat flour tiling when drying for 3 hours
In enamel basin, it is placed into vacuum drying chamber and is dried), obtain wheat flour sample after drying, moisture in wheat flour sample
＜ 1%；
E, it dispenses：Wheat flour sample after step d dryings is sub-packed in the vial of threaded mouth, and covers tightly screw thread
Lid, sealing sample specification is 5g/ bottles, is divided into and fills 500 bottles；
F, irradiation inactivated：The sample of packing is used60Co gamma-ray irradiations inactivate, and dose intensity 7.5kGy, irradiation is gone out
Live time is 2 hours；
G, the sample after step f irradiation inactivateds is vacuum-packed using aluminum foil compound bag, after packaging under the conditions of -20 DEG C
It preserves.
The dependence test of the present embodiment products obtained therefrom wheat flour Analysis on amino acid components standard substance is the same as embodiment 1.Through surveying
Examination, the present embodiment products obtained therefrom are fully able to be used as aminoacid ingredient standard substance.
Embodiment 3：
The preparation method of wheat flour Analysis on amino acid components standard substance of the present invention, the detailed step of the preparation method is such as
Under：
A, it selects：Choose the commercially available wheat flour without any additive；
B, impurity elimination：Wheat flour is first sieved with 100 mesh sieve into carry out screening and removing impurities；
C, degreasing：It will impregnate, impregnated in wheat flour complete wetting to solvent anhydrous ether after step b impurity eliminations
It is sufficiently stirred within every 3 hours in journey once, soaking time is 15 hours, is filtered after immersion, and solvent is filtered, and replaces novel solvent
Anhydrous ether equally impregnates once again, and the wheat flour of degreasing is obtained after immersion treatment；
D, drying：By the wheat flour obtained after step c degreasings, naturally 5 hours shady and cool dry (natural drying is：By degreasing
Wheat flour tiling afterwards is placed in enamel basin to be dried under the conditions of natural environment non-direct sunlight), it is put into after natural drying
It is dried in vacuum drying chamber, drying temperature is 90 DEG C, and drying time is (to be placed in wheat flour tiling when drying and ward off for 4 hours
In ceramic bowl, it is placed into vacuum drying chamber and is dried), obtain wheat flour sample after drying, moisture ＜ in wheat flour sample
1%；
E, it dispenses：Wheat flour sample after step d dryings is sub-packed in the vial of threaded mouth, and covers tightly screw thread
Lid, sealing sample specification is 5g/ bottles, is divided into and fills 500 bottles；
F, irradiation inactivated：The sample of packing is used60Co gamma-ray irradiations inactivate, dose intensity 8kGy, irradiation inactivated
Time is 2 hours；
G, the sample after step f irradiation inactivateds is vacuum-packed using aluminum foil compound bag, after packaging under the conditions of -20 DEG C
It preserves.
The dependence test of the present embodiment products obtained therefrom wheat flour Analysis on amino acid components standard substance is the same as embodiment 1.Through surveying
Examination, the present embodiment products obtained therefrom are fully able to be used as Analysis on amino acid components standard substance.
Claims (7)
1. a kind of preparation method of wheat flour Analysis on amino acid components standard substance, which is characterized in that the preparation method includes
Following steps：
A, it selects：Choose the wheat flour without any additive；
B, impurity elimination：The wheat flour of selection is sieved with 100 mesh sieve into carry out screening and removing impurities；
C, degreasing：It will be impregnated in wheat flour complete wetting to solvent after step b impurity eliminations, every 2~4 hours in soaking process
It is sufficiently stirred once, soaking time is 12~15 hours, is filtered after immersion, and solvent is filtered, and replaces novel solvent and equally soaks again
Bubble is primary, and the wheat flour of degreasing is obtained after immersion treatment；
D, drying：The wheat flour obtained after step c degreasings is naturally shady and cool 4~6 hours dry, it is dry that vacuum is put into after natural drying
It is dried in dry case, obtains wheat flour sample after drying, moisture ＜ 1% in wheat flour sample；
E, it dispenses：Wheat flour sample after step d dryings is sub-packed in vial, and covers tightly threaded cap, seals sample specification
It is 5g/ bottles；
F, irradiation inactivated：The sample of packing is used60Co gamma-ray irradiations inactivate, and dose intensity is 7kGy~10kGy, and irradiation is gone out
Live time is 2 hours；
G, the sample after step f irradiation inactivateds is vacuum-packed using aluminum foil compound bag, is preserved under the conditions of -20 DEG C after packaging.
2. the preparation method of wheat flour Analysis on amino acid components standard substance according to claim 1, it is characterised in that：Step
Solvent described in rapid c is any one of anhydrous ether, petroleum ether, acetone, n-hexane, methanol and ethyl alcohol.
3. the preparation method of wheat flour Analysis on amino acid components standard substance according to claim 2, it is characterised in that：Institute
It is petroleum ether or anhydrous ether to state solvent.
4. the preparation method of wheat flour Analysis on amino acid components standard substance according to claim 1, it is characterised in that：Step
Spontaneously dried described in rapid d is that the wheat flour tiling after degreasing is placed in enamel basin under the conditions of natural environment non-direct sunlight
It is dried.
5. the preparation method of wheat flour Analysis on amino acid components standard substance according to claim 1, it is characterised in that：Step
It is put into vacuum drying chamber and is carried out in drying course described in rapid d, drying temperature is 80~105 DEG C, and drying time is 3~6 small
When.
6. the preparation method of wheat flour Analysis on amino acid components standard substance according to claim 1, it is characterised in that：Step
Vial described in rapid e is the brown bottle of threaded mouth.
7. the preparation method of wheat flour Analysis on amino acid components standard substance according to claim 1, it is characterised in that：Step
Rapid f middle dosage intensity is 7kGy.
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