CN109298122A - A kind of detection method of R- glyceraldehyde acetonide finished product purity - Google Patents
A kind of detection method of R- glyceraldehyde acetonide finished product purity Download PDFInfo
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Abstract
The present invention provides a kind of detection method of R- glyceraldehyde acetonide finished product purity, comprising the following steps: 1) after taking R- glyceraldehyde acetonide finished product that organic solvent dissolution is added, obtains prepare liquid；2) R- glyceraldehyde acetonide standard items and S- glyceraldehyde acetonide standard items are taken, after organic solvent dissolution is added, obtain standard solution；3) respectively by prepare liquid and standard solution, it is detected using GC-FID, it is qualitative to compare retention time progress according to the measured value of standard solution, R- glyceraldehyde acetonide ingredient and S- glyceraldehyde acetonide ingredient in prepare liquid has been determined, and the relative amount of R- glyceraldehyde acetonide and S- glyceraldehyde acetonide in prepare liquid has been determined using peak area normalization method.A kind of detection method of R- glyceraldehyde acetonide finished product purity provided by the invention can be realized being kept completely separate for R- glyceraldehyde acetonide and S- glyceraldehyde acetonide, and method precision, accuracy are good, as a result accurately.
Description
Technical field
The invention belongs to the technical fields of organic compound purity detecting, are related to a kind of R- glyceraldehyde acetonide finished product purity
Detection method, and in particular to R- glyceraldehyde acetonide and S- glyceraldehyde acetonide content in a kind of R- glyceraldehyde acetonide finished product
Detection method.
Background technique
R- glyceraldehyde acetonide, entitled (R)-(+) -2 of chemistry, 2- dimethyl -1,3- dioxy -4- aldehyde radical pentane, is to be used for
The key intermediate of synthesis of chiral drug has good industrial application value.
Currently, it is sweet to generate a small amount of S- since isomerization reaction can occur for the process for preparing R- glyceraldehyde acetonide finished product
Oily aldehyde contracting acetone, and at present existing R- glyceraldehyde acetonide finished product method for detecting purity be gas chromatography, common polarity,
Middle polarity or nonpolar chromatographic column can not separating chiral isomers, make R- glyceraldehyde acetonide finished product purity detecting result not
Accurately.When R- glyceraldehyde acetonide containing S- glyceraldehyde acetonide is further prepared into downstream chipal compounds, isomers
It is difficult to separate, the final quality for influencing chiral drug.Therefore, a kind of easy accurate detection method is established for the contracting of R- glyceraldehyde
The measurement of acetone finished product purity especially effectively detects the content of S- glyceraldehyde acetonide, for R- glyceraldehyde acetonide quality
It monitors significant.
Summary of the invention
In view of the foregoing deficiencies of prior art, the purpose of the present invention is to provide a kind of R- glyceraldehyde acetonide finished products
The detection method of purity can effectively detect R- glyceraldehyde acetonide and S- glyceraldehyde acetonide in R- glyceraldehyde acetonide finished product
Content, so that the purity to R- glyceraldehyde acetonide in R- glyceraldehyde acetonide finished product carries out effective quality control.
In order to achieve the above objects and other related objects, the present invention provides a kind of inspection of R- glyceraldehyde acetonide finished product purity
Survey method, comprising the following steps:
1) sample pre-treatments: after taking R- glyceraldehyde acetonide finished product that organic solvent dissolution is added, prepare liquid is obtained；
2) preparation of standard solution: taking R- glyceraldehyde acetonide standard items and S- glyceraldehyde acetonide standard items, and addition has
After solvent dissolution, standard solution is obtained；
3) sample detection: respectively by the prepare liquid in step 1) and the standard solution in step 2), using gas-chromatography-fire
Flame ionization detector method (GC-FID) is detected, according to the measured value of standard solution compare retention time carry out it is qualitative, really
Determined R- glyceraldehyde acetonide ingredient and S- glyceraldehyde acetonide ingredient in prepare liquid, and using peak area normalization method determined to
Survey the relative amount of R- glyceraldehyde acetonide and S- glyceraldehyde acetonide in liquid.
It preferably, include R- glyceraldehyde acetonide and the contracting of S- glyceraldehyde in step 1), in R- glyceraldehyde acetonide finished product
Acetone.No. CAS of the R- glyceraldehyde acetonide is 15186-48-8.No. CAS of the S- glyceraldehyde acetonide is 22323-
80-4。
Preferably, in step 1), the volume for quality g and the organic solvent addition that the R- glyceraldehyde acetonide finished product is added
The ratio between ml is 2-3:50.
Preferably, in step 2), the R- glyceraldehyde acetonide standard items are by the bright side's new and high technology limited material in Chengdu
The standard items of R- glyceraldehyde acetonide content >=98.0% of company's production.
Preferably, in step 2), the S- glyceraldehyde acetonide standard items are by the limited public affairs of nine ancient cooking vessels chemical (Shanghai) science and technology
The S- glyceraldehyde acetonide standard items of production are taken charge of, also include R- glyceraldehyde acetonide in the standard items.
Preferably, in step 2), the body for quality g and the organic solvent addition that the R- glyceraldehyde acetonide standard items are added
The ratio between product ml is 2-3:50.
Preferably, in step 2), the body for quality g and the organic solvent addition that the S- glyceraldehyde acetonide standard items are added
The ratio between product ml is 2-3:50.
Preferably, step 1) or 2) in, the organic solvent be selected from acetone, methylene chloride, ethyl acetate, toluene, acetonitrile
One of.
Preferably, in step 3), the chromatographic column that the GC-FID method uses is the beta- cyclodextrin chiral selector of chemical bonding
Filler chromatographic column (Coating CP chirasil Dex CB column), column's length 25m, internal diameter 0.25mm, stationary phase
Film thickness is 0.39 μm.
Preferably, in step 3), the sample volume that the GC-FID method uses is 0.1-1.0 μ L.It is highly preferred that the GC-
The sample volume that FID method uses is 0.2 μ L.
Preferably, in step 3), the carrier gas that the GC-FID method uses is high-purity helium, carrier gas purity >=99.999%.
Preferably, in step 3), the flow rate of carrier gas that the GC-FID method uses is 2.0-4.0mL/min.It is highly preferred that institute
The flow rate of carrier gas that GC-FID method uses is stated as 3.0mL/min.
Preferably, in step 3), the input mode that the GC-FID method uses is split sampling, split ratio 50:1.
Preferably, in step 3), the injector temperature that the GC-FID method uses is 250-300 DEG C.It is highly preferred that described
The injector temperature that GC-FID method uses is 280 DEG C.
Preferably, in step 3), the detector that the GC-FID method uses is flame ionization detector (hydrogen flame detection
Device, FID).
Preferably, in step 3), the detector temperature that the GC-FID method uses is 250-300 DEG C.It is highly preferred that described
The detector temperature that GC-FID method uses is 300 DEG C.
Preferably, in step 3), the temperature program of the GC-FID method use are as follows: initial temperature is 40-70 DEG C of holding 1-
3min is warming up to 200 DEG C with the rate of 5-15 DEG C/min, keeps 10-30min.
It is highly preferred that the temperature program that the GC-FID method uses are as follows: initial temperature is 50 DEG C of holding 2min, with 10 DEG C/
The rate of min is warming up to 200 DEG C, keeps 13min.
Preferably, in step 3), the peak area normalization method refers to: by R- glyceraldehyde acetonide finished product sample through GC-FID
After detection, the chromatographic peak area of the R- glyceraldehyde acetonide and S- glyceraldehyde acetonide that calculate separately, and calculate R- glycerol
The sum of the area of each chromatographic peak, obtains total chromatographic peak area in aldehyde contracting acetone finished product.Then, by R- glyceraldehyde acetonide or S-
The chromatographic peak area of glyceraldehyde acetonide obtains R- glyceraldehyde acetonide or S- glyceraldehyde respectively divided by total chromatographic peak area respectively
The chromatographic peak area of contracting acetone accounts for the percentage of total chromatographic peak area, as R- glyceraldehyde acetonide or S- glyceraldehyde acetonide
Relative amount.
Preferably, in step 3), the peak area normalization method is calculated by formula (1), the formula (1) are as follows: wi=
(Ai/ Σ Ai) × 100%, wherein wi be R- glyceraldehyde acetonide finished product sample in R- glyceraldehyde acetonide relative amount or
The relative amount of S- glyceraldehyde acetonide；Ai is the chromatographic peak face of R- glyceraldehyde acetonide in R- glyceraldehyde acetonide finished product sample
Long-pending or S- glyceraldehyde acetonide chromatographic peak area；Σ Ai is total chromatographic peak area in R- glyceraldehyde acetonide finished product sample.
As described above, a kind of detection method of R- glyceraldehyde acetonide finished product purity provided by the invention, using gas phase color
Spectrum-flame ionization detector method (GC-FID) contracts to R- glyceraldehyde acetonide in R- glyceraldehyde acetonide finished product and S- glyceraldehyde
Acetone is detected, and by preferred testing conditions, can be realized sweet as the R- glyceraldehyde acetonide and S- of chiral isomer
Oily aldehyde contracting acetone is kept completely separate, and makes up the deficiency of the existing detection method of the product, method precision, accuracy are good, as a result
Accurately.The detection method is quantified using areas of peak normalization method, and quantitative approach is simple, reproducible.
Detailed description of the invention
Fig. 1 is shown as the gas chromatogram that R- glyceraldehyde acetonide finished product measures in the present invention, wherein a is S- glyceraldehyde
Contracting acetone, b are R- glyceraldehyde acetonide.
Fig. 2 is shown as the gas chromatogram that S- glyceraldehyde acetonide standard items measure in the present invention, wherein a is S- glycerol
Aldehyde contracting acetone, b are R- glyceraldehyde acetonide.
Specific embodiment
The present invention is further explained combined with specific embodiments below, it should be appreciated that these embodiments are merely to illustrate the present invention
Rather than it limits the scope of the invention.
Illustrate embodiments of the present invention below by way of specific specific example, those skilled in the art can be by this specification
Other advantages and efficacy of the present invention can be easily understood for disclosed content.The present invention can also pass through in addition different specific realities
The mode of applying is embodied or practiced, the various details in this specification can also based on different viewpoints and application, without departing from
Various modifications or alterations are carried out under spirit of the invention.
It should be clear that in the following example not specifically dated process equipment or device be all made of conventional equipment in the art or
Device；All pressure values and range all refer to relative pressure.
In addition, it should also be understood that, one or more method and step mentioned in the present invention does not repel before and after the combination step
It can also be inserted into other methods step there may also be other methods step or between these explicitly mentioned steps, unless separately
It is described；It should also be understood that the combination connection relationship between one or more equipment/device mentioned in the present invention is not repelled
The two equipment/devices specifically mentioned before and after the unit equipment/device there may also be other equipment/device or at these it
Between can also be inserted into other equipment/device, unless otherwise indicated.Moreover, unless otherwise indicated, the number of various method steps is only
Identify the convenient tool of various method steps, rather than for the arrangement order of limitation various method steps or limits the enforceable model of the present invention
It encloses, relativeness is altered or modified, and without material changes in technical content, when being also considered as, the present invention is enforceable
Scope.
The reagent and instrument that following embodiment uses are as follows:
1, reagent
R- glyceraldehyde acetonide finished product (commercially available)；R- glyceraldehyde acetonide standard items (R- glyceraldehyde acetonide content >=
98.0%, Chengdu Ming Fang new and high technology Materials Co., Ltd)；S- glyceraldehyde acetonide standard items (glyceraldehyde acetonide containing R-, nine
Ancient cooking vessel chemistry (Shanghai) Science and Technology Ltd.)；Acetone, methylene chloride, ethyl acetate, toluene (analyze pure, Chinese medicines group chemical reagent
Co., Ltd)；Acetonitrile (chromatographically pure, Merck KGaA company).
2, instrument
Agilent 7890A type gas chromatograph (Agilent company of the U.S.) is equipped with flame ionization detector；
Agilent beta- cyclodextrin chiral selector filler chromatographic column (25m × 0.25mm, 0.39 μm) (Agilent company of the U.S.).
Embodiment 1
1, sample pre-treatments
After taking R- glyceraldehyde acetonide finished product that organic solvent dissolution is added, prepare liquid is obtained.Wherein, organic solvent is selected from third
One of ketone, methylene chloride, ethyl acetate, toluene, acetonitrile.R- glyceraldehyde acetonide finished product be added quality g with it is organic molten
The ratio between volume ml that agent is added is 2-3:50.
2, the preparation of standard solution
R- glyceraldehyde acetonide standard items and S- glyceraldehyde acetonide standard items are taken respectively, after organic solvent dissolution is added,
Obtain standard solution.Wherein, the ratio between the volume ml that is added with organic solvent of quality g that R- glyceraldehyde acetonide standard items are added is
2-3:50.The ratio between the volume ml that the quality g and organic solvent that S- glyceraldehyde acetonide standard items are added are added is 2-3:50.It is organic
Solvent is selected from one of acetone, methylene chloride, ethyl acetate, toluene, acetonitrile.
3, it measures
The standard solution that will be prepared in the prepare liquid and step 2 prepared in above-mentioned steps 1, is detected using GC-FID,
It is qualitative to compare retention time progress according to the measured value of standard solution, it is determined that R- glyceraldehyde contracts in R- glyceraldehyde acetonide finished product
Acetone content and S- glyceraldehyde acetonide ingredient, and it has been determined that R- is sweet in R- glyceraldehyde acetonide finished product using peak area normalization method
The relative amount of oily aldehyde contracting acetone and S- glyceraldehyde acetonide.
When specific measurement, the testing conditions of the GC-FID method are as follows: chromatographic column is that the beta- cyclodextrin of chemical bonding is fixed
Phase filling chromatographic column (Coating CP chirasil Dex CB column), column's length 25m, internal diameter 0.25mm are fixed
Phase film thickness is 0.39 μm；Sample volume is 0.1-1.0 μ L；Carrier gas is high-purity helium, carrier gas purity >=99.999%；Flow rate of carrier gas
For 2.0-4.0mL/min；Input mode is split sampling, split ratio 50:1；Injector temperature is 250-300 DEG C；Detector
For flame ionization detector；Detector temperature is 250-300 DEG C；Temperature program are as follows: initial temperature is 40-70 DEG C of holding 1-
3min is warming up to 200 DEG C with the rate of 5-15 DEG C/min, keeps 10-30min.
The peak area normalization method refers to: by R- glyceraldehyde acetonide finished product sample after GC-FID is detected, calculating separately
The chromatographic peak area of obtained R- glyceraldehyde acetonide and S- glyceraldehyde acetonide, and calculate each in R- glyceraldehyde acetonide finished product
The sum of the area of a chromatographic peak, obtains total chromatographic peak area.Then, by R- glyceraldehyde acetonide or the color of S- glyceraldehyde acetonide
Spectral peak area obtains the chromatographic peak face of R- glyceraldehyde acetonide or S- glyceraldehyde acetonide respectively divided by total chromatographic peak area respectively
Product accounts for the percentage of total chromatographic peak area, the as relative amount of R- glyceraldehyde acetonide or S- glyceraldehyde acetonide.
The peak area normalization method is calculated by formula (1), the formula (1) are as follows: wi=(Ai/ Σ Ai) × 100%,
Wherein, wi is the relative amount of R- glyceraldehyde acetonide or the phase of S- glyceraldehyde acetonide in R- glyceraldehyde acetonide finished product sample
To content；Ai is the chromatographic peak area or S- glyceraldehyde acetonide of R- glyceraldehyde acetonide in R- glyceraldehyde acetonide finished product sample
Chromatographic peak area；Σ Ai is total chromatographic peak area in R- glyceraldehyde acetonide finished product sample.
Embodiment 2
1, sample pre-treatments
Take 2.5g R- glyceraldehyde acetonide finished product in 50mL volumetric flask, after methylene chloride dissolved dilution to scale is added,
Obtain prepare liquid.
2, the preparation of standard solution
Take R- glyceraldehyde acetonide standard items 2.5g and S- glyceraldehyde acetonide standard items 2.5g in 50mL volumetric flask respectively
In, after methylene chloride dissolved dilution to scale is added, obtain standard solution.
3, it measures
The standard solution that will be prepared in the prepare liquid and step 2 prepared in above-mentioned steps 1, is detected using GC-FID,
It is qualitative to compare retention time progress according to the measured value of standard solution, it is determined that R- glyceraldehyde contracts in R- glyceraldehyde acetonide finished product
Acetone content and S- glyceraldehyde acetonide ingredient, and it has been determined that R- is sweet in R- glyceraldehyde acetonide finished product using peak area normalization method
The relative amount of oily aldehyde contracting acetone and S- glyceraldehyde acetonide.Specific testing result is shown in Fig. 1,2.By Fig. 1,2 it is found that in the present invention
Method is very good to the separating effect of R- glyceraldehyde acetonide in R- glyceraldehyde acetonide finished product.
When specific measurement, the testing conditions of the GC-FID method are as follows: chromatographic column is that the beta- cyclodextrin of chemical bonding is fixed
Phase filling chromatographic column (Coating CP chirasil Dex CB column), column's length 25m, internal diameter 0.25mm are fixed
Phase film thickness is 0.39 μm；Sample volume is 0.2 μ L；Carrier gas is high-purity helium, carrier gas purity >=99.999%；Flow rate of carrier gas is
3.0mL/min；Input mode is split sampling, split ratio 50:1；Injector temperature is 280 DEG C；Detector is flame ion
Change detector；Detector temperature is 300 DEG C；Temperature program are as follows: initial temperature is 50 DEG C of holding 2min, with the rate of 10 DEG C/min
200 DEG C are warming up to, 13min is kept.
The peak area normalization method refers to: by R- glyceraldehyde acetonide finished product sample after GC-FID is detected, calculating separately
The chromatographic peak area of obtained R- glyceraldehyde acetonide and S- glyceraldehyde acetonide, and calculate each in R- glyceraldehyde acetonide finished product
The sum of the area of a chromatographic peak, obtains total chromatographic peak area.Then, by R- glyceraldehyde acetonide or the color of S- glyceraldehyde acetonide
Spectral peak area obtains the chromatographic peak face of R- glyceraldehyde acetonide or S- glyceraldehyde acetonide respectively divided by total chromatographic peak area respectively
Product accounts for the percentage of total chromatographic peak area, the as relative amount of R- glyceraldehyde acetonide or S- glyceraldehyde acetonide.
The peak area normalization method is calculated by formula (1), the formula (1) are as follows: wi=(Ai/ Σ Ai) × 100%,
Wherein, wi is the relative amount of R- glyceraldehyde acetonide or the phase of S- glyceraldehyde acetonide in R- glyceraldehyde acetonide finished product sample
To content；Ai is the chromatographic peak area or S- glyceraldehyde acetonide of R- glyceraldehyde acetonide in R- glyceraldehyde acetonide finished product sample
Chromatographic peak area；Σ Ai is total chromatographic peak area in R- glyceraldehyde acetonide finished product sample.
Embodiment 3
The R- glyceraldehyde acetonide finished product sample for taking 3 kinds of different manufacturers to produce respectively, number is respectively 1#, 2#, 3#, by real
It applies step 1 preparation test specimens and step 2 in example 2 and prepares standard solution, and be measured by step 3 in embodiment 2, pass through formula
(1) percentage contents of R- glyceraldehyde acetonide and S- glyceraldehyde acetonide in sample are calculated separately.Every kind of sample is surveyed in parallel
5 times fixed, calculated result is shown in Table 1,2.By table 1,2 it is found that this method measures result RSD≤0.05% of R- glyceraldehyde acetonide,
The result RSD < 0.6% of S- glyceraldehyde acetonide is measured, measurement result precision is high, favorable reproducibility.
The precision result (n=5) of 1 sample of table measurement R- glyceraldehyde acetonide
The precision result (n=5) of 2 sample of table measurement S- glyceraldehyde acetonide
Embodiment 4
R- glyceraldehyde acetonide standard items are taken, wherein the content of R- glyceraldehyde acetonide is >=98.0%, by embodiment 2
Step 1 preparation test specimens and step 2 prepare standard solution, and are measured by step 3 in embodiment 2, are calculated by formula (1)
The percentage contents of R- glyceraldehyde acetonide in sample.It is measured in parallel 5 times, calculated result is shown in Table 3.As shown in Table 3, this method
The result RSD < 0.05% of R- glyceraldehyde acetonide is measured, measurement result accuracy is high.
3 method accuracy test result of table confirms data
Embodiment 5
The R- glyceraldehyde acetonide finished product sample that number is 1# in Example 3, by step 1 preparation test in embodiment 2
Sample and step 2 prepare standard solution, then when carrying out detection test specimens using GC-FID, the isothermal of different temperatures setting is respectively adopted
Program, and peak area normalization method is used, the percentage contents of R- glyceraldehyde acetonide in sample are calculated according to formula (1), are surveyed
Surely 4 be the results are shown in Table.Meanwhile the R- glyceraldehyde acetonide finished product sample for 1# will be numbered in embodiment 3 using temperature program measurement
As a result it also enumerates in table 4.
4 different set temperature program(me) measurement result of table
As shown in Table 4, the factors such as separating degree, peak shape and testing time of comprehensive main peak and other impurities component, when this hair
When the bright middle temperature program using optimum condition, main peak can be efficiently separated with other impurities.
Embodiment 6
R- glyceraldehyde acetonide standard items in Example 4 measure implementation using single-point external standard method as standard specimen respectively
Number is respectively the R- glyceraldehyde acetonide finished product sample of 1#, 2#, 3# in example 3, every under chromatographic condition same as Example 3
Kind sample is measured in parallel 5 times, and measurement result is shown in Table 5.
The measurement of 5 single-point external standard method sample of table and precision result (n=5)
By table 5 it is found that the R- of single-point external standard method and the peak area normalization method measurement result in table 1 in table 5 compared with table 1
The percentage contents of glyceraldehyde acetonide are close, but the RSD of the peak area normalization method measurement result in table 1 is substantially better than table 4
In single-point external standard method.As it can be seen that using the quantitative approach of peak area normalization method in the present invention, quantitative approach is simple, not only result
Accuracy is high, and its precision is high, reproducible.
In conclusion a kind of detection method of R- glyceraldehyde acetonide finished product purity provided by the invention, can be realized R-
Glyceraldehyde acetonide is kept completely separate with S- glyceraldehyde acetonide, and method precision, accuracy are good, as a result accurately, quantitative square
Method is simple, reproducible.So the present invention effectively overcomes various shortcoming in the prior art and has high industrial exploitation value
Value.
The above-described embodiments merely illustrate the principles and effects of the present invention, and is not intended to limit the present invention.It is any ripe
The personage for knowing this technology all without departing from the spirit and scope of the present invention, carries out modifications and changes to above-described embodiment.Cause
This, institute is complete without departing from the spirit and technical ideas disclosed in the present invention by those of ordinary skill in the art such as
At all equivalent modifications or change, should be covered by the claims of the present invention.
Claims (10)
1. a kind of detection method of R- glyceraldehyde acetonide finished product purity, comprising the following steps:
1) sample pre-treatments: after taking R- glyceraldehyde acetonide finished product that organic solvent dissolution is added, prepare liquid is obtained；
2) preparation of standard solution: taking R- glyceraldehyde acetonide standard items and S- glyceraldehyde acetonide standard items, is added organic molten
After agent dissolution, standard solution is obtained；
3) sample detection: respectively by the prepare liquid in step 1) and the standard solution in step 2), using gas-chromatography-flame from
Sonization detector method is detected, and it is qualitative to compare retention time progress according to the measured value of standard solution, it is determined that in prepare liquid
R- glyceraldehyde acetonide ingredient and S- glyceraldehyde acetonide ingredient, and R- glycerol in prepare liquid has been determined using peak area normalization method
The relative amount of aldehyde contracting acetone and S- glyceraldehyde acetonide.
2. a kind of detection method of R- glyceraldehyde acetonide finished product purity according to claim 1, which is characterized in that step
1) in, the ratio between the volume ml that the quality g and organic solvent that the R- glyceraldehyde acetonide finished product is added are added is 2-3:50.
3. a kind of detection method of R- glyceraldehyde acetonide finished product purity according to claim 1, which is characterized in that step
Or 2) 1) in, the organic solvent is selected from one of acetone, methylene chloride, ethyl acetate, toluene, acetonitrile.
4. a kind of detection method of R- glyceraldehyde acetonide finished product purity according to claim 1, which is characterized in that step
3) in, the chromatographic column that the GC-FID method uses is the beta- cyclodextrin chiral selector filler chromatographic column of chemical bonding, chromatographic column column
A length of 25m, internal diameter 0.25mm, stationary phase film thickness are 0.39 μm.
5. a kind of detection method of R- glyceraldehyde acetonide finished product purity according to claim 1, which is characterized in that step
3) in, the sample volume that the GC-FID method uses is 0.1-1.0 μ L；The input mode that the GC-FID method uses is is diverted into
Sample, split ratio 50:1.
6. a kind of detection method of R- glyceraldehyde acetonide finished product purity according to claim 1, which is characterized in that step
3) in, the carrier gas that the GC-FID method uses is high-purity helium, carrier gas purity >=99.999%；The load that the GC-FID method uses
Gas velocity is 2.0-4.0mL/min.
7. a kind of detection method of R- glyceraldehyde acetonide finished product purity according to claim 1, which is characterized in that step
3) in, the injector temperature that the GC-FID method uses is 250-300 DEG C.
8. a kind of detection method of R- glyceraldehyde acetonide finished product purity according to claim 1, which is characterized in that step
3) in, the detector temperature that the GC-FID method uses is 250-300 DEG C.
9. a kind of detection method of R- glyceraldehyde acetonide finished product purity according to claim 1, which is characterized in that step
3) in, the temperature program of the GC-FID method use are as follows: initial temperature is 40-70 DEG C of holding 1-3min, with 5-15 DEG C/min's
Rate is warming up to 200 DEG C, keeps 10-30min.
10. a kind of detection method of R- glyceraldehyde acetonide finished product purity according to claim 1, which is characterized in that step
It is rapid 3) in, the peak area normalization method is calculated by formula (1), the formula (1) are as follows: wi=(Ai/ Σ Ai) × 100%,
Wherein, wi is the relative amount of R- glyceraldehyde acetonide or the phase of S- glyceraldehyde acetonide in R- glyceraldehyde acetonide finished product sample
To content；Ai is the chromatographic peak area or S- glyceraldehyde acetonide of R- glyceraldehyde acetonide in R- glyceraldehyde acetonide finished product sample
Chromatographic peak area；Σ Ai is total chromatographic peak area in R- glyceraldehyde acetonide finished product sample.
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| CN112345662A (en) * | 2020-10-22 | 2021-02-09 | 潜江新亿宏有机化工有限公司 | Purity detection method of m-methylbenzyl chloride |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112345662A (en) * | 2020-10-22 | 2021-02-09 | 潜江新亿宏有机化工有限公司 | Purity detection method of m-methylbenzyl chloride |
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