CN107192591A - A kind of preparation method and application of basic orange II standard substance - Google Patents
A kind of preparation method and application of basic orange II standard substance Download PDFInfo
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- CN107192591A CN107192591A CN201710552896.8A CN201710552896A CN107192591A CN 107192591 A CN107192591 A CN 107192591A CN 201710552896 A CN201710552896 A CN 201710552896A CN 107192591 A CN107192591 A CN 107192591A
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- G—PHYSICS
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
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- 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
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- G—PHYSICS
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- 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
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Abstract
The invention discloses a kind of preparation method of basic orange II standard substance, using volume ratio as 4~5：1 ethanol water dissolves raw material basic orange II as solvent at 50 DEG C~80 DEG C, and it is 1 to add volume ratio after dissolving by several times again：1 ethanol water, and be stirred continuously, persistently it is incubated 75 DEG C~85 DEG C, after heat filtering, filtrate is cooled down into room temperature, recrystallized under conditions of being subsequently placed with 4 DEG C, after crystalline solid filtering, drying under the conditions of 60 DEG C, ground sieving produces basic orange II standard substance after mixing, drying；Go out reference materials system using the Developments of certified reference samples prepared, fill the domestic gaps, set up the transmission of quantity value system of measurement process, be that food safety detection and supervision and management provide important technical support.The basic orange II standard substance uncertainty being prepared into is 1%；Available for the basic orange II in the detection system such as food or cosmetics or medicine, it is ensured that the accuracy and comparativity of testing result.
Description
Technical field
The present invention relates to a kind of preparation method and application of basic orange II standard substance.
Background technology
People are good at the organoleptic quality using Pigmentation improvement food, and bright-coloured color and luster not only assigns the pleasant feeling of people's vision,
It can also improve a poor appetite, but some non-food colorings the advantages of its is cheap, strong coloring force, stability are good but because beginning to flow into
Food production line, in recent years, food-safety problem are had no end to disputes, and chemical addition agent is exceeded or frequent hair the problems such as quality
It is raw, great personal injury and property loss are caused, the physical and mental health of people is compromised so that food-safety problem turns into further
The focus of whole society's concern, it is therefore prevented that food pollution, control food quality is prevention disease, ensures people's health
Important measures.
For certain content of material in some sample detection more need standard items as control, current China has also ground
The standard substance for detecting food colour class (such as sunset yellow, amaranth, lemon yellow, famille rose, temptation are red) is made, however,
The Developments of certified reference samples of the violated colouring agent of basic orange II is also in blank stage.Domestic food detection industry is mostly using foreign countries
Relevant criterion product, these standard items are not only expensive, and procurement cycle is long, and do not have traceability mostly, it is impossible to effectively realize
The arbitration of checking and testing result to detection method.
The content of the invention
The technical problems to be solved by the invention be overcome prior art exist above mentioned problem there is provided a kind of basic orange II
The preparation method of standard substance.
Second object of the present invention is to provide the basic orange II standard substance that above-mentioned preparation method is obtained.
Third object of the present invention is to provide a kind of basic orange II solution available for standard substance.
Fourth object of the present invention is to provide a kind of development system for the basic orange II standard substance that above method is obtained.
The 5th purpose of the present invention is to provide the basic orange II standard substance of above method acquisition as standard substance
Using.
The purpose of the present invention is achieved by the following technical programs：
A kind of preparation method of basic orange II standard substance, using volume ratio as 4~5：1 ethanol-water solution is used as solvent
Raw material basic orange II is dissolved, 50 DEG C~80 DEG C of heating makes after its dissolving, and it is 1 that volume ratio is added by several times：1 ethanol-water solution, often
Secondary 10mL~15mL, is stirred continuously simultaneously, is persistently incubated at 75 DEG C~85 DEG C, after heat filtering, filtrate is cooled down into room temperature, then put
Recrystallized, after crystalline solid filtering, dried under the conditions of being placed in 60 DEG C, ground sieving under conditions of putting 4 DEG C, mixed, dry
After produce basic orange II standard substance.
The present invention study route be：The food colour for having important harm to human body is prepared or synthesized, purity rubric is developed
Material, standard liquid.Definite value is carried out to the purity and content of standard substance using chromatography.In the measurements, all instrument used
Device, vessel are calibrated, it is ensured that each link of measurement continual can be traceable to the International System of Units.
Standard substance usually requires that high-purity, and it is constituted and chemical formula is highly consistent and chemically stable, due to reference material
This strict demand of matter, the preparation of standard substance is generally required to be manufactured under conditions of high degree of controlled, this high-purity to reach
Degree, and influence of the impurities to subsequent measurements is avoided as far as possible, therefore the preparation (including purification step) of standard substance will
Complicated many, the physics and chemical property of the invention for basic orange II is prepared than conventional chemical reagent, alkalescence is worked out
The preparation method of the standard substance of orange II, the purity for the basic orange II standard substance that this method is prepared is high, and chemistry, physics
Property is stable.
In some embodiments, during above-mentioned preparation method dissolving raw material basic orange II, the volume ratio of ethanol-water solution is
4：1.
In some embodiments, in above-mentioned preparation method, the time being persistently incubated is 0.3h~0.5h.
In some embodiments, in above-mentioned preparation method, the time of recrystallization is 8h~12h.
The present invention also provides a kind of basic orange II solution available for standard substance, is obtained by any of the above-described kind of preparation method
The basic orange II standard substance obtained is made.
The present invention also provides a kind of development system of the basic orange II standard substance obtained by above-mentioned preparation method, the development
The uniformity testing of system including standard substance, stability test, standard substance definite value, value data statistical analysis and uncertain
Spend the process of analysis.
In some embodiments, stability test point long-time stability are examined and short-term stability is examined, described long-term
Stability test is to examine basic orange II standard substance stability of 30 months by a definite date under condition of storage；The short-term stability
It is to examine basic orange II standard substance one-week stability in the case where temperature is 55 DEG C~65 DEG C of traffic condition.
In some embodiments, analysis on Uncertainty includes uncertainty, the basic orange II standard that definite value experiment is introduced
The uncertainty of the uneven generation of material and the uncertainty of the unstable generation of basic orange II standard substance；The definite value experiment is drawn
The uncertainty entered includes the uncertainty and moisture and the uncertainty of residue experiment introducing that joint definite value is produced.
As a preferred embodiment, the development system includes：
(1) uniformity testing：For certified reference material, it is ensured that the uniformity of material is very important.To be true
Guarantee the quality, improve efficiency, it is to avoid waste, the standard substance candidate of preparation in quantity be distributed into inner wrapping it is previous as to carry out
Even property initial survey.The key link of uniformity initial survey is：Extracting unit number, sampling point, measuring method, minimum sample mass.At random
A number of sample is extracted, is measured using the high test method of precision, determination standard is analyzed by statistical method
Whether material is uniform.
(2) stability test：The stability of standard substance refers to situation about being changed over time by the characteristic quantity of definite value, standard
The stability of material is influenceed by factors such as physics, chemistry and preservation conditions.Study on the stability need to periodically carry out characteristic quantity undetermined
The stability test of value, principle arrangement of the time interval generally according to " being dredged after first close ".The stability of basic orange II standard substance
Divide long-time stability and short-term stability two parts.Long-time stability be carry out under condition of storage 30 months by a definite date stability it is real
Test, short-term stability is one-week study on the stability under simulation southern high-temperature (55 DEG C~65 DEG C) traffic condition.
(3) standard substance definite value：Definite value measurement is the process to standard substance assignment, is also during standard substance is assert
A key link.According to the physicochemical property and analysis method of basic orange II standard substance, 8 laboratory joint definite values are chosen
Method, to standard substance definite value, and to the data in 8 laboratories using Rod Dixon criterion and Grubbs test method to all numbers
According to progress dubious value analysis.
(4) value data statistical analysis：Measurement data is analyzed using statistical method, if assay thinks
There is significant difference, then check measurement method, measuring condition and operating process, and be measured again.Data statistic analysis point
Variance analysis, regression analysis, Rod Dixon criterion and Grubbs test method dubious value analytic approach etc. are not employed.
(5) analysis on Uncertainty：According to《JJG 1006-94 primary standard material technical specifications》With ISO directive/guides 35
The uncertainty to being produced in research process is provided, analysis on Uncertainty is carried out, the uncertainty report of relevant criterion material is completed
Accuse.Uncertainty source mainly has：Part I is the uncertainty that definite value experiment is introduced；Part II is that sample is (i.e. alkaline
Orange II standard substance) uneven generation uncertainty；Part III is the unstable fixed output quota of sample (i.e. basic orange II standard substance)
Raw uncertainty.The uncertainty that definite value experiment is introduced, i.e., the uncertainty produced by joint definite value and moisture and residue are real
Test the uncertainty of introducing.
The basic orange II standard substance that the present invention also provides above-mentioned preparation method acquisition is used as the application of standard substance.
The present invention also provides application of the basic orange II standard substance of above-mentioned preparation method acquisition in detection basic orange II.
Can be specifically basic orange II standard substance detection food, medicine or the cosmetics prepared using the method for the invention
Basic orange II in medium system.
Compared with prior art, the invention has the advantages that：
The present invention obtains the standard substance of basic orange II with the Methods For Purification recrystallized, and carries out definite value to standard substance,
Basic orange II standard substance have developed with the equivalent consistent technology of international metering first, its basic orange II standard substance obtained
Uncertainty be 1%；The development of the standard substance is from state inner detection technique personnel to external import basic orange II standard items
The problem of price height brought and long procurement cycle, and available for the detection system such as food or cosmetics or medicine neutral and alkali orange
II addition, so as to ensure the accuracy and comparativity of testing result.
The Developments of certified reference samples prepared using the inventive method goes out reference materials system, fills the domestic gaps, and sets up
The transmission of quantity value system of measurement process, is that food safety detection and supervision and management provide important technical support.
Brief description of the drawings
Fig. 1 is pigment Developments of certified reference samples route map in food in embodiment of the present invention；
Fig. 2 is basic orange II liquid chromatogram (using DAD detectors)；
Fig. 3 is the infrared spectrum for developing basic orange II purity rubric material；
Fig. 4 is the basic orange II standard IR spectrogram searched in SDBS picture libraries；
Fig. 5 is the basic orange II high resolution mass spec figure developed；
Fig. 6 is the mass spectrum retrieval result of basic orange II.
Embodiment
The present invention is expanded on further with reference to Figure of description and specific embodiment.These embodiments are merely to illustrate this
Invention rather than limitation the scope of the present invention.The experimental method of unreceipted actual conditions in lower example embodiment, generally according to this
Field normal condition or the condition advised according to manufacturer.Unless otherwise defined, all specialties and science used in text
Term is identical with meaning familiar to the person skilled in the art.
Embodiment 1
The preparation of basic orange II standard substance：Using alcohol-water, (volume ratio is 4：1) solution is solvent, is added on electric hot plate
Heat makes after its dissolving to 80 DEG C, then it is 1 to add volume ratio by several times：1 ethanol-water solution, every time 10~15mL, and constantly stirring
Mix, be incubated 20min, filtering, filtrate recrystallizes 8h under conditions of 4 DEG C, is dried after filtering, and ground sieving is produced after mixing
Candidate criteria material.
First, the purity of candidate criteria material
Purity analysis is carried out to candidate criteria material principal component using liquid chromatography area normalization method, liquid chromatogram is such as
Shown in Fig. 2, as a result show：The purity of basic orange II is 99.5%.
Also the moisture and residue of basic orange II are analyzed simultaneously, moisture is obtained by test and residue content is distinguished
For 0.15%, 0.14%.
Because liquid chromatogram Par value basic orange II purity rubric material will consider the influence of sample moisture and residue, thus should
The purity of method definite value：
2nd, the Structural Identification of candidate criteria material
The experiment such as infrared analysis, high resolution mass spec will be carried out by basic orange II purity material after purification.Obtain infrared spectrum
(Fig. 3) and standard IR spectrogram (Fig. 4), high resolution mass spec (Fig. 5) and retrieval result (Fig. 6), are drawn a conclusion by comparison diagram：
Basic orange II purity material infrared spectrum after purification is consistent with standard spectrogram contrast, judges principal component for Basic Orange
Ⅱ；High resolution mass spec retrieval matching degree is 99.1%, it was demonstrated that purity material is really basic orange II.
3rd, the definite value experiment of candidate criteria material
(1) standard substance definite value
Except inventor carries out definite value, the also suitable laboratory association of selective power to preparation-obtained candidate criteria material
Definite value is helped, every Laboratory Instruments is qualified by legal metrological service before, and each laboratory is from whole samples
3 packagings are randomly selected, 1~3 increment is arbitrarily taken out from every bottle, with hplc grade methanol when solvent prepares test fluid, are used
Liquid chromatography measures basic orange II purity rubric material.The experimental result of 8 laboratory definite values is listed in Table 1 below.
The basic orange II purity rubric agents in combination definite value result of table 1
Above-mentioned data are analyzed using Pauta criterion, found without suspicious data.Therefore, using the overall average in 8 laboratories
It is worth the result as joint definite value.
Overall average is as follows：
Dubious value analysis is carried out to all data using Rod Dixon criterion and Grubbs test method, dubious value is not found.Tool
Body analysis process is as follows：
1. use Rod Dixon (Dixon) criterion
According to the data of table 1, by arranging from small to large：
99.25<99.40<99.41<99.41<99.46<99.59<99.82<99.84
Because of n=8, then
r8＜ r1, r1＜ D (a, n), D (a, n)=0.608 of tabling look-up to obtain,
Illustrate that this group of data are as good as constant value.
2. differentiated using Grubbs test method
Arithmetic average：
Experiment with computing standard deviation：S=0.211
Calculate each residual errorFor：- 0.27, -0.12, -0.11, -0.11, -0.06,0.07,0.30,0.32
Look into Grubbs test method critical value：G (0.05,8)=2.032
Therefore, illustrate to be as good as constant value.
(2) uniformity testing
Reference standard material technology specification, respectively from having dispensed and being numbered with the basic orange II purity sample of number by
According to end to end, middle numbering respectively randomly select 15 bottles of samples.
The sample about 10mg that precise is extracted, is configured to solution, determines pure using liquid chromatogram-area normalization method
Degree, actual conditions：Using liquid chromatogram DAD detectors, chromatographic column is C18 (5.0 μm, 4.6mm*250mm) posts or similar pillar,
Methanol and 0.02mol/L ammonium acetate are mobile phase, are matched as 65：35, flow velocity is 1.0mL/min, and Detection wavelength is 407nm.
Then the parallel sample introduction of every bottle of sample 3 times, the average value measured every time carry out variance point as the result of Evaluation for Uniformity to it
Analysis.
Instrument and measurer, are first all examined and determine, and confirm that instrument is in normal working condition, and ensure instrument and amount
Has the traceability of measurement.
The basic orange II purity rubric material homogeneity test data of table 2 and result
The basic orange II purity rubric material uniformity results variance analysis of table 3
Data can be obtained in table：
Fα(ν1,ν2)=2.037, α=0.05
F<F α show that notable difference is not present in sample room.
BecauseThe standard deviation that now uniformity is produced is calculated as follows：
The standard deviation of method measurement：
It can be seen that from calculating：It is critical that the statistic F values of basic orange II purity sample measurement result are less than uniformity testing
Value F α：2.037, it was demonstrated that the basic orange II purity sample is uniform.
(3) stability test
The stability of standard substance refers to situation about being changed over time by the characteristic quantity of definite value, the stability of standard substance by
The influence of the factors such as physics, chemistry and preservation condition.Need to carry out it with the high analysis method of precision for a long time periodically
Investigate to determine the relative stable time limit.This project establishing criteria material technology specification, in line with preceding tight rear thin principle, to alkalescence
Orange II purity rubric material stability has carried out long-time stability and short-term stability is investigated.Investigate stability and use liquid chromatogram
Method, using area normalization method, is compared measurement in different time intervals.
Short-term stability refers to stability of the standard substance in transportation under traffic condition.In order to investigate transport bar
Part considers southern hot weather to the stability influence of standard substance, simulates traffic condition, randomly selects 6
Bottle sample, is respectively placed under traffic condition ((60 ± 5) DEG C)) ((4 ± 1) DEG C) preservation under (in incubator) and customary storage conditions
In one week, two kinds of different conditions of contrast are to its stability influence (by taking 60 DEG C of measurement temperature as an example).
The long-time stability of basic orange II purity rubric material are that inspection basic orange II standard substance is under condition of storage
The stability of 30 months phases, investigation the results are shown in Table 4~5, and the short-term stability of basic orange II purity rubric material is investigated result and seen
Table 7.
The basic orange II purity rubric material long-time stability experimental data of table 4
The basic orange II purity rubric material long-time stability experimental data the results of analysis of variance of table 5
| The free degree | SS | MS | F values | sig.F | |
| Regression analysis | 1 | 0.040 | 0.040 | 0.775 | 0.419 |
| Residual error | 5 | 0.260 | 0.052 | ||
| Amount to | 6 | 0.300 |
The Regression Analysis Result of the basic orange II purity rubric material long-time stability experimental data of table 6
| Coefficient | Standard error | T- statistics | P values | Lower limit 95% | The upper limit 95% | |
| Intercept | 99.45 | 0.143 | 698.06 | 1.15E-13 | 99.09 | 99.82 |
| Slope | 0.007 | 0.009 | 0.880 | 0.419 | -0.014 | 0.029 |
Because not a kind of physical/chemical model can truly describe the mechanism of degradation of the candidate criteria sample, therefore adopt
With straight line empirically model, the time is represented with x, the value of basic orange II purity rubric material is represented with y, be fitted to one it is straight
Line, then the slope of straight line be：
In formula：
Intercept is calculated by following formula：
The standard deviation of point on straight line is calculated by following formula：
Its square root s=0.2280% is taken, the uncertainty of slope is：
The free degree f=n-2=4 and p=0.95 (95% confidence level) t distribution factors are equal to 2.78.Due to | b1| ＜
t0.95,n-2·s(b1), therefore slope is inapparent.Unstability is not thus observed, that is, is shown in 30 months, the recurrence is
Inapparent (sig.F=0.3567>0.05) obvious trend does not occur for the value for, being basic orange II purity rubric material
Property change, this illustrates the stability that we take condition of storage to be effectively guaranteed basic orange II purity rubric material value.
The basic orange II purity rubric material short-term stability experimental data (60 DEG C) of table 7
Same statistical analysis is carried out to the measurement data under the conditions of two kinds, standard substance value does not have under the conditions of finding two kinds
There are generation significant changes.
Investigated by long-time stability and short-term stability, be 30 months in, basic orange II purity rubric thing in stationary phase
Matter has good stability, and significant change does not occur for value, and the candidate criteria material that the present invention is prepared is in condition of storage and fortune
Stability is ensure that under the conditions of defeated well.
(4) analysis on Uncertainty
According to《JJG 1006-94 primary standard material technical specifications》Regulation with ISO directive/guides 35 in research process to producing
Raw uncertainty, carries out analysis on Uncertainty, completes the uncertainty report of relevant criterion material.Uncertainty source is main
Have：Part I is the uncertainty that definite value experiment is introduced；Part II is that sample (i.e. basic orange II standard substance) is uneven
The uncertainty of generation；Part III is the uncertainty of sample (i.e. basic orange II standard substance) unstable generation.Definite value is real
Test the uncertainty of introducing, i.e., the uncertainty that the uncertainty produced by joint definite value and moisture and residue experiment are introduced.
The uncertainty that the experiment of 4.1 definite values is introduced, i.e., the uncertainty produced by joint definite value and moisture and residue experiment
The uncertainty of introducing
4.1.1 uncertainty (the u that joint definite value is introducedJoint)
According to ISO directive/guides 35, the uncertainty of Duo Jia laboratories cooperation definite value can be estimated using variance analysis.It is fixed
The result that value result one-way analysis of variance is obtained is listed in table 8 and table 9.
The one-way analysis of variance result that table 8 is obtained by the data of table 1
The one-way analysis of variance result that table 9 is obtained by the data of table 1
| Difference source | SS | df | MS | F | P-value | F crit |
| Between group | 0.961 | 7 | 0.137 | 224.12 | 9.37E-15 | 2.657 |
| In group | 0.010 | 16 | 6.3E-4 | |||
| Amount to | 0.971 | 23 |
The uncertainty of overall average is calculated as below：
4.1.2 the uncertainty that moisture measurement is introduced
According to the data of moisture measurement, the R=0.1% of measure, n=6 (table look-up c=2.53) calculate water using range method
Separate into partial uncertainty be：
4.1.3 uncertainty (the u that residue test is introducedResidue)
The data measured according to residue, the R=0.07% of measure, n=6 (table look-up c=2.53) calculate residual using range method
Slag introduce partial uncertainty be：uResidue=R/c=0.03%
4.1.4 definite value introduces total uncertainty (uDefinite value)
Standard uncertainty (the u that 4.2 uniformities are producedbb)
Uniformity uses the purity of basic orange II can by uniformity some numerical results to compare parameter (data are shown in Table 2)
Know, the standard deviation between sample bottle produced by inhomogeneities must be incorporated into total uncertainty.Therefore, sample room is uneven
Standard deviation：
ubb≈ 0.013%
Uncertainty (the u that 4.3 stability are introducedIts)
According to the experimental data of basic orange II long-time stability, (table 4 and regression variance result (table 5,6) understand to divide by stable
Property interpretation of result understand that the uncertainty contribution of the long-time stability of term of validity t=30 months is：
uIts=sbT=8.5 × 10-3× 30=0.255%
The total uncertainty of 4.4 standard substances
Expanded uncertainty：U95=k × uAlways=2 × 0.272%=0.54% ≈ 1.0%
The definite value result of basic orange II purity rubric material is:W=(99.2 ± 1.0) %, k=2.
Its result shows：Candidate criteria material that the present embodiment is prepared is not known as 1%.
Embodiment 2
The preparation of basic orange II standard substance：Using alcohol-water, (volume ratio is 4：1) solution is solvent, is added on electric hot plate
Heat makes after its dissolving to 75 DEG C, then it is 1 to add volume ratio by several times：1 ethanol-water solution, 10~15mL, and constantly stirring every time
Mix, be incubated 30min, filtering, filtrate recrystallizes 8h under conditions of 4 DEG C, is dried after filtering, and ground sieving is produced after mixing
Candidate criteria material.
Above-described is only some embodiments of the present invention.For the person of ordinary skill of the art, not
On the premise of departing from the invention design, various modifications and improvements can be made, these belong to the protection model of the present invention
Enclose.
Claims (10)
1. a kind of preparation method of basic orange II standard substance, it is characterised in that using volume ratio as 4~5：1 ethanol-water solution
Raw material basic orange II is dissolved as solvent, 50 DEG C~80 DEG C of heating makes after its dissolving, and it is 1 that volume ratio is added by several times：1 ethanol-
The aqueous solution, each 10mL~15mL, is stirred continuously simultaneously, is persistently incubated at 75 DEG C~85 DEG C, after heat filtering, by filtrate cooling chamber
Temperature, is recrystallized under conditions of being subsequently placed with 4 DEG C, after crystalline solid filtering, is dried under the conditions of being placed in 60 DEG C, ground sieving,
Basic orange II standard substance is produced after mixing, drying.
2. the preparation method of basic orange II standard substance according to claim 1, it is characterised in that dissolving raw material Basic Orange
When II, the volume ratio of ethanol-water solution is 4：1.
3. the preparation method of basic orange II standard substance according to claim 1, it is characterised in that the time being persistently incubated
For 0.3h~0.5h.
4. the preparation method of basic orange II standard substance according to claim 1, it is characterised in that the time of recrystallization is
8h~12h.
5. a kind of basic orange II solution available for standard substance, it is characterised in that be as described in any one of Claims 1-4
The basic orange II standard substance that method is obtained is made.
6. a kind of development system of the basic orange II standard substance obtained by any one of Claims 1-4 methods described, its feature
It is, including the uniformity testing of standard substance, stability test, standard substance definite value, value data statistical analysis and not true
The process of fixed degree analysis.
7. the development system of basic orange II standard substance according to claim 6, it is characterised in that the stability test
Long-time stability are divided to examine and short-term stability inspection, the long-time stability inspection is inspection basic orange II standard substance in storage
The stability of 30 months by a definite date under the conditions of depositing；The short-term stability be examine basic orange II standard substance temperature be 55 DEG C~
One-week stability under 65 DEG C of traffic condition.
8. the development system of basic orange II standard substance according to claim 6, it is characterised in that the uncertainty point
Analysis includes uncertainty, the uncertainty of the uneven generation of basic orange II standard substance and the basic orange II mark that definite value experiment is introduced
The uncertainty of the quasi- unstable generation of material；The uncertainty that the definite value experiment is introduced includes the uncertain of joint definite value generation
The uncertainty that degree and the experiment of moisture and residue are introduced.
9. the basic orange II standard substance that any one of Claims 1-4 methods described is obtained is used as the application of standard substance.
10. the basic orange II standard substance that any one of Claims 1-4 methods described is obtained answering in detection basic orange II
With.
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| CN112816283A (en) * | 2020-12-30 | 2021-05-18 | 国家烟草质量监督检验中心 | Preparation method of tobacco specific N-nitrosamine standard substance |
| CN113075183A (en) * | 2021-03-26 | 2021-07-06 | 广东省计量科学研究院（华南国家计量测试中心） | DPA solution relative fluorescence emission intensity standard substance and preparation method and application thereof |
| CN113176125A (en) * | 2021-04-30 | 2021-07-27 | 中国计量科学研究院 | Linear range standard substance of full-automatic biochemical analyzer and preparation method and application thereof |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112816283A (en) * | 2020-12-30 | 2021-05-18 | 国家烟草质量监督检验中心 | Preparation method of tobacco specific N-nitrosamine standard substance |
| CN113075183A (en) * | 2021-03-26 | 2021-07-06 | 广东省计量科学研究院（华南国家计量测试中心） | DPA solution relative fluorescence emission intensity standard substance and preparation method and application thereof |
| CN113075183B (en) * | 2021-03-26 | 2022-02-22 | 广东省计量科学研究院（华南国家计量测试中心） | DPA solution relative fluorescence emission intensity standard substance and preparation method and application thereof |
| CN113176125A (en) * | 2021-04-30 | 2021-07-27 | 中国计量科学研究院 | Linear range standard substance of full-automatic biochemical analyzer and preparation method and application thereof |
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| CN107192591B (en) | 2018-08-07 |
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