CN107132302A - A kind of external standard method calculates the assessment method of drugs constituent content assay uncertainty - Google Patents
A kind of external standard method calculates the assessment method of drugs constituent content assay uncertainty Download PDFInfo
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Abstract
The invention discloses a kind of method for evaluating drugs constituent content assay uncertainty, methods described includes：The foundation of measurement result calculation formula and mathematical modeling, uncertainty source analysis, the quantization of partial uncertainty, the calculating of combined standard uncertainty, the calculating of expanded uncertainty, the expression of measurement result.By means of the invention it is also possible to accurately reflect the main source of influence uncertainty, more structurally sound inspection measurement result can be provided.
Description
Technical field
The invention belongs to forensic science drugs of abuse field, it is related to external standard method calculating drugs constituent content assay not true
Surely the assessment method spent.It is applied to point using liquid chromatogram and gas chromatographic technique measurement drugs content results uncertainty
Analysis.
Background technology
At present, the drug issue being on the rise turns into global disaster.The body for spreading unchecked the directly harm people of drugs
Heart health, and bring grave danger to economic growth and social progress.Therefore, forensic science illicit drugs inspection magnitude tracing body is set up
System, improves drugs composition measurement technique, it is ensured that the reliability and comparativity of measurement result, sets up the shared and mutual of measurement data
Recognize, accurately and reliably evidence is provided for court, it has also become countries in the world drugs appraisal organization question of common concern.
Drugs composition measurement technique and traceability guarantee are an organic wholes, are core measurement capabilities in section of court
Learn the important embodiment of drugs ingredient amount fields of measurement.Master body is measured with a measuring system or measuring instrument
When, the result of measurement often deviates actual value to a certain extent.Produce these deviation the reason for include systematic uncertainty,
Environment random noise even self-defect of exemplar etc..In practice, these deviations are mathematically often described as one not
Determine that angle value, that is, the uncertain angle value determine the scope where the actual value of master body to a certain extent.Nowadays,
The evaluation of uncertainty and method for expressing uniformly have become an important indicator in international scientific exchange and trade.World mark
Standardization is organized in its revision《Calibration and the General Requirement of testing laboratory's ability》(ISO17025) clearly proposed in, laboratory
Each certificate or report, it is necessary to comprising about calibrate and test result uncertainty evaluation explanation, uncertainty is pair
The quantitatively characterizing of measurement result quality, the availability of measurement result is heavily dependent on the size of its uncertainty.So
Uncertain accurate calculating and expression are most important for effective expressed intact of measurement result.
The content of the invention
When carrying out component content analysis to drugs using the measuring systems such as gas-chromatography or liquid chromatogram or measuring instrument, no
Produce deviation to a certain extent with can avoiding, be mathematically represented as uncertain angle value；It is an object of the invention to be China's administration of justice
Evaluation department provides drugs content probation report a kind of method for analyzing uncertainty, by setting up uncertainty calculation mathematics
Model, the source of each uncertainty of analysis, expansion uncertainty expression, realize uncertain accurate analysis and conjunction in measurement process
Reason expression.
To reach above-mentioned purpose, the present invention uses following technical proposals：
A kind of external standard method calculates the assessment method of drugs constituent content assay uncertainty, comprises the following steps：Survey
The foundation of amount result calculation formula and mathematical modeling, uncertainty source analysis, the quantization of partial uncertainty, synthetic standards are not
The calculating of degree of certainty, the calculating of expanded uncertainty, the expression of measurement result.
Above-mentioned external standard method calculates the assessment method of drugs constituent content assay uncertainty, for gas chromatography or
Drugs constituent content in liquid chromatography for measuring drugs sample, its quantitative math-model is：
In formula：W --- the percentage composition of drugs component, % in sample；
V1--- the first constant volume of sample solution, mL；
V2--- from V1In pipette sample solution volume, mL；
V3--- by V2Solvent volume, mL are added during dilution；
A --- the chromatographic peak area average value of drugs component in sample solution；
A0--- the chromatographic peak area average value of drugs component in standard working solution；
Co--- the concentration of drugs component, mg/mL in standard working solution；
M --- for the weighing weight of the drugs sample of measure, mg.
Above-mentioned external standard method calculates the assessment method of drugs constituent content assay uncertainty, uncertainty source bag
Include：The uncertainty u that measurement reproducibility is introduced0, standard working solution CoUncertainty u (the C of introducingo), the drugs sample for measure
Uncertainty u (m), the first constant volume V of sample that this weighing weight m is introduced1Introduce uncertainty u (V1), from V1In pipette V2
Uncertainty u (the V that the sample solution of volume is introduced2), V in sample solution dilution2And V3The uncertainty u of introducing
(V2+3), drugs component color spectrum peak area response A in standard working solution0Drugs component in the uncertainty of introducing, sample solution
The uncertainty that chromatographic peak area response A is introduced.
Above-mentioned external standard method calculates the assessment method of drugs constituent content assay uncertainty, under the conditions of repeatability,
Duplicate measurements n time is started since sampling to same sample, if result is being averaged of determining for n times, measurement reproducibility introducing it is not true
Surely component u is spent0Calculation formula be：
Above-mentioned external standard method calculates the assessment method of drugs constituent content assay uncertainty, is prepared from standard reserving solution
Standard working solution C prepared by the dilution of standard working solutionoUncertainty u (the C of introducingo) computational mathematics model is：
In formula：C0--- the concentration of drugs component, mg/mL in standard working solution；
C --- the concentration of drugs component, mg/mL in standard reserving solution；
V01--- pipette the volume of standard reserving solution, mL；
V02--- the volume of standard working solution is prepared, i.e., single graticule volumetric flask volume, mL.
Above-mentioned external standard method calculates the assessment method of drugs constituent content assay uncertainty, the drugs sample for measure
This quality m introduces uncertainty u (m) according to the balance limits of error and assumes that distributed rectangular can be calculated：
Above-mentioned external standard method calculates the assessment method of drugs constituent content assay uncertainty, the initial constant volume of sample
V1Introduce uncertainty u (V1) consider the influence calibrated with temperature to volume and assume that distributed rectangular can be calculated：u(V1)
=0.0578mL；From V1In pipette V2Uncertainty u (the V that the sample solution of volume is introduced2)=0.0074V2mL；Sample solution
V in dilution2And V3The uncertainty of introducingN ' is addition
The number of times of solvent.
Above-mentioned external standard method calculates drugs in the assessment method of drugs constituent content assay uncertainty, standard working solution
Component chromatogram honeybee area response value A0The uncertainty of introducing is not considered；Drugs component color composes honeybee area response in sample solution
The uncertainty that value A is introduced is not considered.
Above-mentioned external standard method calculates the assessment method of drugs constituent content assay uncertainty, combined standard uncertainty
Calculation formula be：
The calculation formula of expanded uncertainty is：U=k × uc(w) %；Under 95% fiducial probability, Coverage factor k=2 is taken；
Measurement result is expressed as w% ± U%, k=2.
Beneficial effects of the present invention are as follows：
Heretofore described method provides drugs content probation report a kind of analysis not for judicial expertise department of China
The method of degree of certainty, and can provide accurate, reasonable, mutual trust, effectively expressing mode by theory and practice proof.Available for state
Uncertainty calculation method in interior drugs Content Test report comes from present invention, and theory and practice is proved in the present invention
The calculating of uncertainty is rationally, reliably.
Brief description of the drawings
The embodiment to the present invention is described in further detail below in conjunction with the accompanying drawings.
Fig. 1 evaluates the method flow diagram of uncertainty.
Embodiment
In order to illustrate more clearly of the present invention, the present invention is done further with reference to preferred embodiments and drawings
It is bright.Similar part is indicated with identical reference in accompanying drawing.It will be appreciated by those skilled in the art that institute is specific below
The content of description is illustrative and be not restrictive, and should not be limited the scope of the invention with this.
Embodiment 1
The present embodiment is the uncertainty evaluation method of drugs assay result in case sample of being involved in drug traffic, it is adaptable to used
Gas chromatography or liquid chromatography detection, external standard method calculate the uncertainty evaluation of drugs content results.To case inspection of being involved in drug traffic
Drugs component in material is extracted with solvent, is analyzed using gas-chromatography (GC) or liquid chromatogram (HPLC), uses external standard
Method is quantified.
The foundation of measurement result calculation formula and mathematical modeling
The quantitative math-model of drugs constituent content is in gas chromatography or liquid chromatography for measuring drugs sample：
In formula：W --- the percentage composition of drugs component, % in sample；
V1--- the first constant volume of sample solution, mL；
V 2--- from V1In pipette sample solution volume, mL；
V3--- by V2Solvent volume, mL are added during dilution；
A --- the chromatographic peak area average value of drugs component in sample solution；
A0--- the chromatographic peak area average value of drugs component in standard working solution；
Co--- the concentration of drugs component, mg/mL in standard working solution；
M --- for the weighing weight of the drugs sample of measure, mg.
Uncertainty source analysis
Source is analyzed from measurement process and mathematical modeling：
1st, the uncertainty u that measurement reproducibility is introduced0
2nd, standard working solution CoUncertainty u (the C of introducingo) --- prepare standard working solution from from standard reserving solution
Dilution
3rd, the drugs sample for measure weighs the uncertainty u (m) that weight m is introduced --- weigh drugs from balance
The process of sample
4th, the first constant volume V of sample1Introduce uncertainty u (V1)
5th, from V1In pipette V2Uncertainty u (the V that the sample solution of volume is introduced2)
6th, V in sample solution dilution2And V3Uncertainty u (the V of introducing2+3)
7th, drugs component color spectrum peak area response A in standard working solution0The uncertainty of introducing
8th, the uncertainty that drugs component color spectrum peak area response A is introduced in sample solution
The quantization of partial uncertainty
1st, the uncertainty u that measurement reproducibility is introduced0
Under the conditions of repeatability, duplicate measurements n times is started since sampling to same sample, if result is being averaged of determining for n times,
The uncertainty that then measurement reproducibility is introduced
2nd, standard working solution CoUncertainty u (Co)
Drugs solution reference material (standard reserving solution) V is accurately pipetted using pipettor01ML, is placed in volume for V02ML's
In single graticule volumetric flask, scale is settled to solvent, standard working solution is diluted to.Mathematical modeling is：
In formula：C0--- the concentration of drugs component, mg/mL in standard working solution；
C --- the concentration of drugs component, mg/mL in standard reserving solution；
V01--- pipette the volume of standard reserving solution, mL；
V 02--- the volume of standard working solution is prepared, i.e., single graticule volumetric flask volume, mL.
(1) the uncertainty u (C) that drugs concentration of component C is introduced in standard reserving solution
State's quality inspection amount letter characteristic and uncertainty explanation or mark according to the national standard material grading certificate middle finger number of delimiting the organizational structure
The explanation of dispatching from the factory of quasi- material, concentration is 1.00mg/mL national drugs solution reference material, and its expanded uncertainty is
± 0.03mg/mL, it is assumed that be normal distribution, being then converted into standard uncertainty is：
(2) standard reserving solution V is pipetted01Uncertainty u (the V that mL is introduced01)
A. the influence u to volume is calibrated1(V01)
According to People's Republic of China (PRC) national metrological verification regulations JJG 646-2006, pipettor is in 20 DEG C of normal temperature
When, its capacity allowable error should meet the requirement of table 1.
The pipettor capacity allowable error of table 1.
1000 μ L standard reserving solutions are pipetted into volumetric flask for 1000 μ L pipettor using the nominal capacity of assay approval,
It is assumed that distributed rectangular, then being converted into standard uncertainty is：
B. influence u of the temperature to volume2(V01)
Temperature control is tested at 20 ± 8 DEG C, but the organic solvent coefficient of expansion is 1.0 × 10-3/ DEG C, therefore the Volume Changes produced
For ± (V01×8×1.0×10-3)=± 0.008V01ML, it is assumed that temperature change is distributed rectangular, then：
By above-mentioned V01Partial uncertainty synthesis：
(3) V is prepared02Uncertainty u (the V that mL standard working solutions are introduced02)
A. the influence u to volume is calibrated1(V02)
According to People's Republic of China (PRC) national metrological verification regulations JJG 196-2006, single graticule volumetric flask is in normal temperature
At 20 DEG C, its capacity allowable error should meet the requirement of table 2.
The single graticule volumetric flask capacity allowable error of table 2.
The use of nominal capacity is 10mL, through examining and determine single graticule volumetric flask for B grades, capacity franchise is ± 0.040mL, it is assumed that
For distributed rectangular, then being converted into standard uncertainty is：
B. influence u of the temperature to volume2(V02)
Temperature control is tested at 20 ± 8 DEG C, but the organic solvent coefficient of expansion is 1.0 × 10-3/ DEG C, therefore the Volume Changes produced
For ± (V02×8×1.0×10-3)=± 0.008V02=± 0.08mL, it is assumed that temperature change is distributed rectangular, then：
By above-mentioned V02Partial uncertainty synthesis：
Summary,
u(C0)=urel(C0)×C0=0.0176 × 0.1=0.0018
3rd, the drugs sample quality m for measure introduces uncertainty u (m)
According to People's Republic of China (PRC) national metrological verification regulations JJG 1036-2008, work bar at -10 DEG C~+40 DEG C
Under part, table 3 should be met to the balance weighing limits of error and required.
The electronic balance limits of error of table 3.
For I grade of electronic balance that precision is ten a ten thousandths and assay approval, actual graduation value d=0.01mg, calibrating point
Angle value e=10d=0.1mg, in 0≤m≤5000mg range of weighing, the limits of error are ± 0.5e=± 0.5 × 0.1mg=
±0.05mg.Weigh and repeat the requirement that sexual deviation equally satisfaction is no more than respective loads limits of error absolute value, take maximum
For 0.05mg.It is assumed that distributed rectangular, being converted into standard uncertainty is：
Net weight, by weighing operation gained twice, is once tare weight mtare, another time is gross weight mgross.It is independent sight because weighing each time
Result is surveyed, therefore is calculated twice.Weighing sample introducing standard uncertainty is：
4th, the initial constant volume V of sample1Introduce uncertainty u (V1)
With 2 standard working solution CoUncertainty u (Co) in (2) pipette standard reserving solution V01ML introduces standard uncertainty
u(V01) evaluation.
10mL solvents are pipetted into test tube for 10mL pipettor using assay approval and nominal capacity, it is assumed that for rectangle point
Cloth, then：
Calibrate the influence to volume
Influence of the temperature to volume
By above-mentioned V1Partial uncertainty synthesis：
The partial uncertainty for pipetting generation for 1 time is u (V1)=0.0578
The partial uncertainty for pipetting generation n times is
5th, from V1In pipette V2Uncertainty u (the V that the sample solution of volume is introduced2)
With 7.2 standard working solution CoUncertainty u (Co) in (2) pipette standard reserving solution V01The standard that mL is introduced is not true
Surely u (V are spent01) evaluation.
u(V2)=0.0074V2mL
6th, V in sample solution dilution2And V3Uncertainty u (the V of introducing2+3)
In dilution first constant volume sample solution V is pipetted using nominal capacity for 1000 μ L pipettor2=1mL, is adopted
The pipettor for being 10mL with nominal capacity adds solvent dilution, and solvent 10mL is added every time, and addition number of times is n ', then solvent is added
Measure V3The uncertainty evaluation of introducing is with 4, the initial constant volume V of sample1Introduce uncertainty u (V1)。
The partial uncertainty that the secondary addition solvents of n ' are produced is
7th, drugs component color spectrum honeybee area response value A in standard working solution0The uncertainty of introducing
Due in measurement indirectly repeated calculatings to contain all influence factors in whole measurement process small at random
The standard uncertainty that drugs component color spectral peak area is introduced in comprehensive function, therefore standard working solution should be refused to repeat to consider.
8th, the uncertainty that drugs component color spectrum honeybee area response value A is introduced in sample solution
Due in measurement indirectly repeated calculatings to contain all influence factors in whole measurement process small at random
The standard uncertainty that drugs component color spectral peak area is introduced in comprehensive function, therefore sample liquid should be refused to repeat to consider.
The calculating of combined standard uncertainty
Numerical value and partial uncertainty table in the sample of table 4 in drugs constituent content continuous mode
By each partial uncertainty synthesis in table 4
If the measurement result of drugs constituent content is w% in sample,
uc(w)=w × ucrel(w)
The calculating of expanded uncertainty
U=k × uc(w) % (under 95% fiducial probability, taking Coverage factor k=2)
Measurement result is represented
The content of drugs component in sample：W% ± U%, k=2.
Embodiment 2
A kind of external standard method calculates the assessment method of drugs constituent content assay uncertainty, comprises the following steps：
(1) drugs constituent content in drugs sample is determined using gas chromatography, setting up quantitative math-model is：
In formula：W --- the percentage composition of drugs component, % in sample；
V1--- the first constant volume of sample solution, 20mL；
V2--- from V1In pipette sample solution volume, 1mL；
V3--- by V2Solvent volume, 20mL are added during dilution；
A --- the chromatographic peak area average value 50 of drugs component in sample solution；
A0--- the chromatographic peak area average value 50 of drugs component in standard working solution；
Co--- the concentration of drugs component, 0.1mg/mL in standard working solution；
M --- for the weighing weight of the drugs sample of measure, mg.
Parallel sampling is weighed 6 times, and weight (mg) is respectively 50.01,50.02,50.03,49.97,49.98,49.99；Sample
The chromatographic peak area of drugs component is respectively 50.01,50.02,50.03,49.97,49.98,49.99 in this solution；Survey twice
The chromatographic peak area for measuring drugs component in standard working solution is respectively 49.99,50.01.
It can be calculated, the percentage composition of drugs component is 84% in sample.
(2) analysis uncertainty source includes：The uncertainty u that measurement reproducibility is introduced0, standard working solution CoIntroduce
Uncertainty u (Co), the drugs sample for measure weighs uncertainty u (m), the first constant volume V of sample that weight m is introduced1
Introduce uncertainty u (V1), from V1In pipette V2Uncertainty u (the V that the sample solution of volume is introduced2), sample solution diluted
V in journey2And V3The uncertainty u of introducing
(V2+3), drugs component color spectrum peak area response A in standard working solution0In the uncertainty of introducing, sample solution
The uncertainty that drugs component chromatographic peak area response value A is introduced.
(3) the uncertainty u that measurement reproducibility is introduced is calculated0。
Under the conditions of repeatability, as a result duplicate measurements 6 times since sampling to same sample are that result is 6 surveys respectively
Fixed is averaged, the partial uncertainty u introduced according to measurement reproducibility0Calculation formulaWithIt can be calculated u0=0
(4) the standard working solution Co for calculating the dilution preparation for preparing standard working solution from standard reserving solution is introduced not
Degree of certainty u (Co), mathematical modeling is
In formula：C0--- the concentration of drugs component, 0.1mg/mL in standard working solution；
C --- the concentration of drugs component, 1mg/mL in standard reserving solution；
V01--- pipette the volume of standard reserving solution, mL；
V02--- the volume of standard working solution is prepared, i.e., single graticule volumetric flask volume, mL.
Understand accordingly, standard working solution Co uncertainty u (Co) has following three part to introduce, i.e. (a) standard reserving solution
The uncertainty u (C) that middle drugs concentration of component C is introduced, (b) pipettes the uncertainty u (V of standard reserving solution V01mL introducings01) and
(c) V is prepared02Uncertainty u (the V that mL standard working solutions are introduced02).Wherein, standard reserving solution V is pipetted01It is uncertain that mL is introduced
Spend u (V01) and preparation V02Uncertainty u (the V that mL standard working solutions are introduced02) consider calibration and influence of the temperature to volume.
It can be calculated,
u(C0)=0.0018
(5) calculate for measure drugs sample quality m introduce uncertainty u (m) according to the balance limits of error simultaneously
It is assumed that distributed rectangular can be calculated
(6) the initial constant volume V of sample is calculated1Introduce uncertainty u (V1) consider the shadow of calibration and temperature to volume
Ring and assume that distributed rectangular can be calculated：
u(V1)=0.0578mL.
(7) calculate from V1In pipette V2Uncertainty u (the V that the sample solution of volume is introduced2)=0.0074V2mL。
(8) V in sample solution dilution is calculated2And V3The uncertainty of introducing
(9) drugs component color spectrum honeybee area response value A in standard working solution is calculated0The uncertainty of introducing is not considered.
(10) uncertainty that drugs component color spectrum honeybee area response value A is introduced in sample solution is calculated not consider.
(11) calculation formula of calculating combined standard uncertainty is
uc(w)=1.676
(12) calculation formula of expanded uncertainty is
U=k × uc(w) %=3.4 (under 95% fiducial probability, taking Coverage factor k=2)
(13) measurement result is expressed as 84.0% ± 3.4%, k=2.
In summary, the present invention to drugs content by gas chromatograph or liquid chromatogram external standard method to being measured foundation
Mathematical modeling, is fully analyzed the every uncertainty factor source that may be introduced in operating process, and is carried out reasonable, accurate
Really quantify, by calculating Composite Seismogram and expanded uncertainty, realize accurate, the property recognized each other to drugs assay result
Expression, is that judicial expertise mechanism and judicial organs provide reasonable, believable reference frame.
Obviously, the above embodiment of the present invention is only intended to clearly illustrate example of the present invention, and is not pair
The restriction of embodiments of the present invention, for those of ordinary skill in the field, may be used also on the basis of the above description
To make other changes in different forms, all embodiments can not be exhaustive here, it is every to belong to this hair
Row of the obvious changes or variations that bright technical scheme is extended out still in protection scope of the present invention.
Claims (9)
1. a kind of external standard method calculates the assessment method of drugs constituent content assay uncertainty, comprise the following steps：Measurement
As a result the foundation of calculation formula and mathematical modeling, uncertainty source analysis, the quantization of partial uncertainty, synthetic standards are not true
Surely the calculating spent, the calculating of expanded uncertainty, the expression of measurement result.
2. a kind of external standard method according to claim 1 calculates the evaluation side of drugs constituent content assay uncertainty
Method, it is characterised in that for drugs constituent content, its quantitative mathematical in gas chromatography or liquid chromatography for measuring drugs sample
Model is：
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In formula：W --- the percentage composition of drugs component, % in sample；
V1--- the first constant volume of sample solution, mL；
V2--- from V1In pipette sample solution volume, mL；
V3--- by V2Solvent volume, mL are added during dilution；
A --- the chromatographic peak area average value of drugs component in sample solution；
A0--- the chromatographic peak area average value of drugs component in standard working solution；
Co--- the concentration of drugs component, mg/mL in standard working solution；
M --- for the weighing weight of the drugs sample of measure, mg.
3. a kind of external standard method according to claim 2 calculates the evaluation side of drugs constituent content assay uncertainty
Method, it is characterised in that uncertainty source includes：The uncertainty u that measurement reproducibility is introduced0, standard working solution CoIntroduce not
Degree of certainty u (Co), the drugs sample for measure weighs uncertainty u (m), the first constant volume V of sample that weight m is introduced1Draw
Enter uncertainty u (V1), from V1In pipette V2Uncertainty u (the V that the sample solution of volume is introduced2), sample solution dilution
Middle V2And V3Uncertainty u (the V of introducing2+3), drugs component color spectrum peak area response A in standard working solution0What is introduced is not true
The uncertainty that drugs component color spectrum peak area response A is introduced in fixed degree, sample solution.
4. a kind of external standard method according to claim 3 calculates the assessment method of drugs constituent content assay uncertainty, it is special
Levy and be, under the conditions of repeatability, duplicate measurements n times is started since sampling to same sample, if result is being averaged of determining for n times, measure
The partial uncertainty u that repeatability is introduced0Calculation formula be：
5. a kind of external standard method according to claim 4 calculates the evaluation side of drugs constituent content assay uncertainty
Method, it is characterised in that standard working solution C prepared by the dilution for preparing standard working solution from standard reserving solutionoIntroduce not
Degree of certainty u (Co) computational mathematics model is：
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In formula：C0--- the concentration of drugs component, mg/mL in standard working solution；
C --- the concentration of drugs component, mg/mL in standard reserving solution；
V01--- pipette the volume of standard reserving solution, mL；
V02--- the volume of standard working solution is prepared, i.e., single graticule volumetric flask volume, mL；
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<mo>(</mo>
<msub>
<mi>V</mi>
<mn>02</mn>
</msub>
<mo>)</mo>
</mrow>
</mrow>
<msub>
<mi>V</mi>
<mn>02</mn>
</msub>
</mfrac>
<mo>&rsqb;</mo>
</mrow>
<mn>2</mn>
</msup>
</mrow>
</msqrt>
<mo>;</mo>
<mo>.</mo>
</mrow>
6. a kind of external standard method according to claim 5 calculates the evaluation side of drugs constituent content assay uncertainty
Method, it is characterised in that the drugs sample quality m for measure introduces uncertainty u (m) according to the balance limits of error and vacation
Determine distributed rectangular can be calculated：
<mrow>
<mi>u</mi>
<mrow>
<mo>(</mo>
<mi>m</mi>
<mo>)</mo>
</mrow>
<mo>=</mo>
<msqrt>
<mrow>
<mn>2</mn>
<mo>&times;</mo>
<msup>
<mn>0.0409</mn>
<mn>2</mn>
</msup>
</mrow>
</msqrt>
<mo>=</mo>
<mn>0.0579</mn>
<mo>;</mo>
</mrow>
<mrow>
<msub>
<mi>u</mi>
<mrow>
<mi>r</mi>
<mi>e</mi>
<mi>l</mi>
</mrow>
</msub>
<mrow>
<mo>(</mo>
<mi>m</mi>
<mo>)</mo>
</mrow>
<mo>=</mo>
<mfrac>
<mrow>
<mi>u</mi>
<mrow>
<mo>(</mo>
<mi>m</mi>
<mo>)</mo>
</mrow>
</mrow>
<mi>m</mi>
</mfrac>
<mo>=</mo>
<mfrac>
<mn>0.0579</mn>
<mi>m</mi>
</mfrac>
<mo>.</mo>
</mrow>
7. a kind of external standard method according to claim 6 calculates the evaluation side of drugs constituent content assay uncertainty
Method, it is characterised in that the initial constant volume V of sample1Introduce uncertainty u (V1) consider the shadow of calibration and temperature to volume
Ring and assume that distributed rectangular can be calculated：
From V1In pipette V2It is uncertain that the sample solution of volume is introduced
Spend u (V2)=0.0074V2ML,V in sample solution dilution2And V3The uncertainty of introducingN ' is the number of times for adding solvent,
8. a kind of external standard method according to claim 7 calculates the evaluation side of drugs constituent content assay uncertainty
Method, it is characterised in that drugs component color spectrum honeybee area response value A in standard working solution0The uncertainty of introducing is not considered；Sample
The uncertainty that drugs component color spectrum honeybee area response value A is introduced in this solution is not considered.
9. a kind of external standard method according to claim 8 calculates the evaluation side of drugs constituent content assay uncertainty
Method, it is characterised in that the calculation formula of combined standard uncertainty is：
<mrow>
<msub>
<mi>u</mi>
<mi>c</mi>
</msub>
<mrow>
<mo>(</mo>
<mi>w</mi>
<mo>)</mo>
</mrow>
<mo>=</mo>
<mi>w</mi>
<mo>&times;</mo>
<msqrt>
<mrow>
<msup>
<mrow>
<mo>(</mo>
<mfrac>
<msub>
<mi>u</mi>
<mn>0</mn>
</msub>
<mi>w</mi>
</mfrac>
<mo>)</mo>
</mrow>
<mn>2</mn>
</msup>
<mo>+</mo>
<msubsup>
<mi>u</mi>
<mrow>
<mi>r</mi>
<mi>e</mi>
<mi>l</mi>
</mrow>
<mn>2</mn>
</msubsup>
<mrow>
<mo>(</mo>
<msub>
<mi>C</mi>
<mn>0</mn>
</msub>
<mo>)</mo>
</mrow>
<mo>+</mo>
<msubsup>
<mi>u</mi>
<mrow>
<mi>r</mi>
<mi>e</mi>
<mi>l</mi>
</mrow>
<mn>2</mn>
</msubsup>
<mrow>
<mo>(</mo>
<mi>m</mi>
<mo>)</mo>
</mrow>
<mo>+</mo>
<msubsup>
<mi>u</mi>
<mrow>
<mi>r</mi>
<mi>e</mi>
<mi>l</mi>
</mrow>
<mn>2</mn>
</msubsup>
<mrow>
<mo>(</mo>
<msub>
<mi>V</mi>
<mn>1</mn>
</msub>
<mo>)</mo>
</mrow>
<mo>+</mo>
<msubsup>
<mi>u</mi>
<mrow>
<mi>r</mi>
<mi>e</mi>
<mi>l</mi>
</mrow>
<mn>2</mn>
</msubsup>
<mrow>
<mo>(</mo>
<msub>
<mi>V</mi>
<mn>2</mn>
</msub>
<mo>)</mo>
</mrow>
<mo>+</mo>
<msubsup>
<mi>u</mi>
<mrow>
<mi>r</mi>
<mi>e</mi>
<mi>l</mi>
</mrow>
<mn>2</mn>
</msubsup>
<mrow>
<mo>(</mo>
<msub>
<mi>V</mi>
<mrow>
<mn>2</mn>
<mo>+</mo>
<mn>3</mn>
</mrow>
</msub>
<mo>)</mo>
</mrow>
</mrow>
</msqrt>
<mo>;</mo>
</mrow>
The calculation formula of expanded uncertainty is：U=k × uc(w) %；Under 95% fiducial probability, Coverage factor k=2 is taken；Measurement
As a result w% ± U%, k=2 are expressed as.
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