CN107192591B - 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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- CN107192591B CN107192591B CN201710552896.8A CN201710552896A CN107192591B CN 107192591 B CN107192591 B CN 107192591B CN 201710552896 A CN201710552896 A CN 201710552896A CN 107192591 B CN107192591 B CN 107192591B
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- G—PHYSICS
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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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Abstract
The invention discloses a kind of preparation methods of basic orange II standard substance, with volume ratio for 4~5：1 ethanol water dissolves raw material basic orange II as solvent at 50 DEG C~80 DEG C, and it is 1 that volume ratio is added after dissolving by several times again：1 ethanol water, and be stirred continuously, persistently keep the temperature 75 DEG C~85 DEG C, after heat filtering, filtrate is cooled down into room temperature, is recrystallized under conditions of being subsequently placed with 4 DEG C, after crystalline solid filtering, it is dry under the conditions of 60 DEG C, ground sieving, up to basic orange II standard substance after mixing, drying；Go out reference materials system using the Developments of certified reference samples being prepared, fill the domestic gaps, establish the transmission of quantity value system of measurement process, important technical support is provided for food safety detection and supervision and management.The basic orange II standard substance uncertainty being prepared into is 1%；It can be used for detecting the basic orange II in food or the systems such as cosmetics or drug, ensure 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, however certain non-food colorings are but because the advantages that its is cheap, strong coloring force, stability are good begins to flow into
The frequent hair for the problems such as food production line, in recent years, food-safety problem are had no end to disputes, and chemical addition agent is exceeded or quality
It is raw, great personal injury and property loss are caused, compromises the physical and mental health of people so that food-safety problem becomes further
The hot spot of whole society's concern, it is therefore prevented that food pollution, control food quality is to prevent disease, ensure people's health
Important measures.
Need standard items for the detection of certain content of material in some sample China has also been ground at present as a contrast more
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 colorant of basic orange II is also in blank stage.Domestic food detection industry mostly uses external
Relevant criterion product, these standard items are not only expensive, and procurement cycle is long, and do not have traceability mostly, can not effectively realize
The arbitration of verification and testing result to detection method.
Invention content
The technical problem to be solved by the present invention is to overcome the above problem of the existing technology, a kind of basic orange II is provided
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 obtains.
Third object of the present invention is to provide a kind of basic orange II solution can be used 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 the above method obtains.
Fifth object of the present invention is to provide the basic orange II standard substances of above method acquisition as standard substance
Using.
The purpose of the present invention is what is be achieved by the following technical programs：
A kind of preparation method of basic orange II standard substance, with volume ratio for 4~5：1 ethanol-water solution is as solvent
Raw material basic orange II is dissolved, after 50 DEG C~80 DEG C of heating makes it dissolve, it is 1 that volume ratio is added by several times：1 ethanol-water solution, often
Secondary 10mL~15mL, is stirred continuously simultaneously, and filtrate after heat filtering, is cooled down room temperature, then put by lasting heat preservation at 75 DEG C~85 DEG C
It is recrystallized under conditions of setting 4 DEG C, dry under the conditions of being placed in 60 DEG C after crystalline solid filtering, ground sieving, mixing, drying
Afterwards up to 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
Substance, standard solution.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, and ensure that measuring each link continual can be traceable to the International System of Units.
Standard substance usually requires that high-purity, and chemical stabilization highly consistent with chemical formula is formed, due to reference substance
This strict demand of matter, the preparation of standard substance is generally required to be manufactured under conditions of high degree of controlled, to reach this high-purity
Degree, and influence of the impurities to subsequent measurements is avoided as far as possible, therefore the preparation (including purification step) of standard substance is wanted
Complicated more than preparing for conventional chemical reagent, the present invention is directed to the physics and chemical property of basic orange II, works out alkalinity
The purity of the preparation method of the standard substance of orange II, the basic orange II standard substance that this method is prepared is high, and chemistry, physics
Property is stablized.
In some embodiments, when 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 persistently kept the temperature 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 can be used for standard substance, 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 developments
System includes the uniformity testing of standard substance, stability test, standard substance definite value, value data statistical analysis and uncertain
Spend the process of analysis.
In some embodiments, stability test divides long-time stability to examine and is examined with short-term stability, described long-term
Stability test is to examine basic orange II standard substance 30 months by a definite date stability 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 introduces
The uncertainty of the uncertainty and the unstable generation of basic orange II standard substance of the uneven generation of substance；The definite value experiment is drawn
The uncertainty entered includes the uncertainty that joint definite value generates and moisture and the uncertainty that residue experiment introduces.
As a preferred embodiment, the development system includes：
(1) uniformity testing：For certified reference material, ensure that the uniformity of substance is very important.It is true
Guarantee the quality, improve efficiency, avoid wasting, 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, measurement method, minimum sample mass.At random
A certain number of samples are extracted, are measured using the high test method of precision, the standard of determination is analyzed by statistical method
Whether substance is uniform.
(2) stability test：The stability of standard substance refers to standard the case where being changed over time by the characteristic quantity of definite value
The stability of substance is influenced 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 are the stability realities carried out under condition of storage 30 months by a definite date
It tests, 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 during assert to the process and standard substance of standard substance assignment
A key link.According to the physicochemical property and analysis method of basic orange II standard substance, chooses 8 laboratories and combine definite value
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 inspection result thinks
Significant difference then checks measurement method, measuring condition and operating process, and is measured again.Data statistic analysis point
Variance analysis, regression analysis, Rod Dixon criterion and Grubbs test method dubious value analytic approach etc. are not used.
(5) analysis on Uncertainty：According to《JJG 1006-94 primary standard substance technical specifications》With ISO directive/guides 35
It provides the uncertainty to being generated in research process, carries out analysis on Uncertainty, complete the uncertainty report of relevant criterion substance
It accuses.Uncertainty source mainly has：First part is the uncertainty that definite value experiment introduces；Second part 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 introduces, i.e., the uncertainty generated by joint definite value and moisture and residue are real
Test the uncertainty of introducing.
Application the present invention also provides the basic orange II standard substance of above-mentioned preparation method acquisition as standard substance.
The present invention also provides application of the basic orange II standard substance of above-mentioned preparation method acquisition in detecting basic orange II.
The specific can be that the basic orange II standard substance detection food, drug or the cosmetics that are 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 is had developed with the equivalent consistent technology of international metering for the first time, the 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 caused price height and procurement cycle length, and can be used for detecting food or the systems such as cosmetics or drug neutral and alkali orange
II addition, to ensure the accuracy and comparativity of testing result.
Go out reference materials system using the Developments of certified reference samples that the method for the present invention is prepared, fill the domestic gaps, establishes
The transmission of quantity value system of measurement process provides important technical support for food safety detection and supervision and management.
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 substance；
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.
Specific implementation mode
The present invention is further explained with specific embodiment with reference to the accompanying drawings of the specification.These embodiments are merely to illustrate this
It invents rather than limits the scope of the invention.Test method without specific conditions in lower example embodiment, usually according to this
Field normal condition or the condition suggested according to manufacturer.Unless otherwise defined, all professions and science used in text
Term is identical as meaning familiar to the person skilled in the art.
Embodiment 1
The preparation of basic orange II standard substance：With alcohol-water (volume ratio 4：1) solution is solvent, is added on electric hot plate
After heat makes it dissolve to 80 DEG C, then it is 1 that volume ratio is added by several times：1 ethanol-water solution, 10~15mL every time, and constantly stir
It mixes, keeps the temperature 20min, filtering, filtrate recrystallizes 8h under conditions of 4 DEG C, dry after filtering, ground sieving, after mixing to obtain the final product
Candidate criteria substance.
One, the purity of candidate criteria substance
Purity analysis is carried out to candidate criteria substance principal component using liquid chromatography area normalization method, liquid chromatogram is such as
Shown in Fig. 2, the results showed that：The purity of basic orange II is 99.5%.
Also the moisture of basic orange II and residue are analyzed simultaneously, moisture is obtained by test and residue content is distinguished
It is 0.15%, 0.14%.
Because liquid chromatogram Par value basic orange II purity rubric substance will consider the influence of sample moisture and residue, thus should
The purity of method definite value：
Two, the Structural Identification of candidate criteria substance
The experiments 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 comparison, judges principal component for Basic Orange
Ⅱ；It is 99.1% that high resolution mass spec, which retrieves matching degree, it was demonstrated that purity material is really basic orange II.
Three, the definite value experiment of candidate criteria substance
(1) standard substance definite value
In addition to inventor carries out definite value, the also comparable laboratory association of selective power to preparation-obtained candidate criteria substance
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, from 1~3 increment is arbitrarily taken out in every bottle, with hplc grade methanol when solvent prepares test fluid, use
Liquid chromatography measures basic orange II purity rubric substance.The experimental result of 8 laboratory definite values is listed in Table 1 below.
1 basic orange II purity rubric agents in combination definite value result of table
Above-mentioned data are analyzed using Pauta criterion, are 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, does not find dubious value.Tool
Body analytic process is as follows：
1. using Rod Dixon (Dixon) criterion
According to 1 data of table, 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), table look-up to obtain D (a, n)=0.608,
Illustrate that this group of data are no different constant value.
2. being 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 no different constant value.
(2) uniformity testing
Reference standard material technology specification, respectively from dispensed and be numbered in the basic orange II purity sample of number by
According to end to end, intermediate number respectively randomly select 15 bottles of samples.
The sample about 10mg that precise extracts, is configured to solution, is measured using liquid chromatogram-area normalization method pure
Degree, actual conditions：Using liquid chromatogram DAD detectors, chromatographic column is C18 (5.0 μm, 4.6mm*250mm) columns or similar pillar,
The ammonium acetate of methanol and 0.02mol/L are mobile phase, and it is 65 to match：35, flow velocity 1.0mL/min, Detection wavelength 407nm.
The parallel sample introduction of every bottle of sample 3 times, the average value measured every time is as Evaluation for Uniformity as a result, then carrying out variance point 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 measured.
2 basic orange II purity rubric substance homogeneity test data of table and result
3 basic orange II purity rubric substance uniformity results variance analysis of table
It can be obtained by data 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 uniformity generates at this time is calculated as follows：
The standard deviation that method measures：
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 the case where 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.It needs to carry out it with the high analysis method of precision prolonged regular
It investigates to determine the opposite stabilization time limit.This project establishing criteria material technology specification, in line with preceding next thin principle, to alkalinity
Orange II purity rubric material stability has carried out long-time stability and short-term stability is investigated.It investigates stability and uses liquid chromatogram
Measurement is compared in interval in different times using area normalization method in method.
Short-term stability refers to stability of the standard substance in transportational process under traffic condition.In order to investigate transport item
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 comparison are to its stability influence (by taking 60 DEG C of measuring temperature as an example).
The long-time stability of basic orange II purity rubric substance 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 substance is investigated result and seen
Table 7.
4 basic orange II purity rubric substance long-time stability experimental data of table
5 basic orange II purity rubric substance long-time stability experimental data the results of analysis of variance of table
| Degree of freedom | SS | MS | F values | sig.F | |
| Regression analysis | 1 | 0.040 | 0.040 | 0.775 | 0.419 |
| Residual error | 5 | 0.260 | 0.052 | ||
| It amounts to | 6 | 0.300 |
The Regression Analysis Result of 6 basic orange II purity rubric substance long-time stability experimental data of table
| 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 |
Due to there is no a kind of physical/chemical model that 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 substance 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%, the uncertainty of slope is taken to be：
The t distribution factors of degree of freedom f=n-2=4 and p=0.95 (95% confidence level) 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, which is
Inapparent (sig.F=0.3567>0.05) apparent trend does not occur for the magnitude for, being basic orange II purity rubric substance
Property variation, this illustrates that our taken conditions of storage are effectively guaranteed the stability of basic orange II purity rubric substance magnitude.
7 basic orange II purity rubric substance short-term stability experimental data (60 DEG C) of table
Same statistical analysis is carried out to the measurement data under the conditions of two kinds, standard substance magnitude does not have under the conditions of finding two kinds
There are generation significant changes.
It is investigated by long-time stability and short-term stability, is 30 months in stationary phase, basic orange II purity rubric object
Matter has good stability, and significant change does not occur for magnitude, and the candidate criteria substance that the present invention is prepared is in condition of storage and fortune
Stability is well ensured under the conditions of defeated.
(4) analysis on Uncertainty
According to《JJG 1006-94 primary standard substance 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 substance.Uncertainty source is main
Have：First part is the uncertainty that definite value experiment introduces；Second part 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 of the uncertainty and moisture and residue experiment introducing that are generated by joint definite value.
The uncertainty that the experiment of 4.1 definite values introduces, i.e., the uncertainty generated by joint definite value and moisture and residue are tested
The uncertainty of introducing
4.1.1 uncertainty (the u that joint definite value introducesJoint)
According to ISO directive/guides 35, variance analysis can be used to be estimated in the uncertainty of the laboratories Duo Jia cooperation definite value.It is fixed
The result that value result one-way analysis of variance obtains 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 | |||
| It amounts to | 0.971 | 23 |
The uncertainty of overall average calculates as follows：
4.1.2 the uncertainty that moisture measurement introduces
According to the data of moisture measurement, the R=0.1% of measurement, 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 introducesResidue)
According to the data that residue measures, the R=0.07% of measurement, n=6 (table look-up c=2.53) are calculated 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 generatebb)
Uniformity uses the purity of basic orange II can by uniformity some numerical results to compare parameter (data are shown in Table 2)
Know, standard deviation caused by inhomogeneities must be incorporated into total uncertainty between sample bottle.Therefore, sample room is uneven
Standard deviation：
ubb≈ 0.013%
Uncertainty (the u that 4.3 stability introduceIts)
According to the experimental data of basic orange II long-time stability, (table 4 and regression variance result (table 5,6) point are by stablizing
Property interpretation of result it is found that the uncertainty contribution of term of validity t=30 months long-time stability 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 substance is:W=(99.2 ± 1.0) %, k=2.
Itself the result shows that：Not knowing for the candidate criteria substance that the present embodiment is prepared is 1%.
Embodiment 2
The preparation of basic orange II standard substance：With alcohol-water (volume ratio 4：1) solution is solvent, is added on electric hot plate
After heat makes it dissolve to 75 DEG C, then it is 1 that volume ratio is added by several times：1 ethanol-water solution, 10~15mL every time, and constantly stir
It mixes, keeps the temperature 30min, filtering, filtrate recrystallizes 8h under conditions of 4 DEG C, dry after filtering, ground sieving, after mixing to obtain the final product
Candidate criteria substance.
Above-described is only some embodiments of the present invention.For those of ordinary skill in the art, not
Under the premise of being detached from the invention design, various modifications and improvements can be made, these belong to the protection model of the present invention
It encloses.
Claims (6)
1. a kind of preparation method of basic orange II standard substance, which is characterized in that with volume ratio for 4 ~ 5：1 ethanol-water solution
Raw material basic orange II is dissolved as solvent, after 50 DEG C ~ 80 DEG C of heating makes it dissolve, it is 1 that volume ratio is added by several times：1 alcohol-water
Solution, the mL of 10 mL ~ 15, are stirred continuously simultaneously every time, lasting heat preservation at 75 DEG C ~ 85 DEG C, the time persistently kept the temperature be 0.3h~
Filtrate after heat filtering, is cooled down room temperature, is recrystallized under conditions of being subsequently placed with 4 DEG C by 0.5h, after crystalline solid filtering, is placed in
It is dry under the conditions of 60 DEG C, ground sieving, up to candidate basic orange II standard substance after mixing, drying；
Purity analysis：Purity analysis is carried out to candidate basic orange II standard substance using liquid chromatogram-area normalization method, is confirmed
Whether its purity is not less than 99.2%；
Structural Identification：Infrared analysis, high resolution mass spec experiment are carried out, structure mirror is carried out to candidate basic orange II standard substance
It is fixed, confirm whether the candidate criteria substance is basic orange II；
Uniformity testing：From dispensed and be numbered in the candidate basic orange II standard substance of number according to end to end, intermediate compile
No less than 15 bottles of samples number are randomly selected, 10 mg of sample that precise extracts is configured to solution, using liquid chromatogram-area
Normalization method measures purity；The parallel sample introduction of every bottle of sample 3 times, the average value measured every time is as Evaluation for Uniformity as a result, right
Statistical analysis is carried out to it afterwards, whether confirmatory sample measurement result is statistically notable, and confirms candidate basic orange II mark
Whether quasi- substance is uniform；
Stability test：Candidate basic orange II standard substance sample is respectively placed in 60 ± 5 DEG C of incubator and 4 ± 1 DEG C normal
It advises and preserves a week under condition of storage, be placed under 4 ± 1 DEG C of customary storage conditions and preserve 30 months, judge whether there is shakiness
Whether qualitative and stability is up to standard；
Analysis on Uncertainty：Uncertainty, the Basic Orange that definite value experiment introduces are carried out to candidate basic orange II standard substance sample
The analysis on Uncertainty of the uncertainty and the unstable generation of basic orange II standard substance of the uneven generation of II standard substance；
If purity analysis, Structural Identification, uniformity testing, stability test and analysis on Uncertainty are satisfied by requirement, it is made
Basic orange II standard substance.
2. the preparation method of basic orange II standard substance according to claim 1, which is characterized 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, which is characterized in that the time of recrystallization is
8h~12h.
4. a kind of basic orange II solution can be used for standard substance, which is characterized in that be described in any one of claims 1 to 3
The basic orange II standard substance that method obtains is made.
5. application of the basic orange II standard substance that any one of claims 1 to 3 the method obtains as standard substance.
6. application of the basic orange II standard substance that any one of claims 1 to 3 the method obtains in detecting basic orange II.
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| 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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