CN104198423B - Method for rapidly detecting content of 2,3-dibenzyl succinic acid - Google Patents
Method for rapidly detecting content of 2,3-dibenzyl succinic acid Download PDFInfo
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- CN104198423B CN104198423B CN201410428407.4A CN201410428407A CN104198423B CN 104198423 B CN104198423 B CN 104198423B CN 201410428407 A CN201410428407 A CN 201410428407A CN 104198423 B CN104198423 B CN 104198423B
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- succinic acid
- dibenzyl succinic
- dibenzyl
- potassium hydroxide
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Abstract
The invention relates to a method for rapidly detecting the content of 2,3-dibenzyl succinic acid. The method comprises the following steps: (1) confirming the maximum absorption wavelength by virtue of scanning of a 2,3-dibenzyl succinic acid ultraviolet absorption spectrum; (2) preparing a 2,3-dibenzyl succinic acid standard sample solution; (3) acquiring a 2,3-dibenzyl succinic acid standard curveinear regression equation; (4) preparing a to-be-detected 2,3-dibenzyl succinic acid sample; (5) detecting 2,3-dibenzyl succinic acid by using ultraviolet light; and (6) calculating the concentration of 2,3-dibenzyl succinic acid. By adopting the method, the content of 2,3-dibenzyl succinic acid can be detected, so that the yield and quality of a later reaction product can be controlled. The method is simple in operation, low in detection cost, accurate in detection result and applicable to rapid detection on a midbody in the production process.
Description
Technical field
The present invention relates to the assay method of content of material, specifically one kind rapidly and efficiently detect 2,3- dibenzyl fourth two
The new method of acid content.
Background technology
2,3- dibenzyl succinic acid are the intermediate of synthetic vitamin h, and w factor, also known as biotin, coenzyme r, is fat
The material indispensable with protein homergy, is that a kind of maintenance animal grows and water necessary to intact animal's function naturally
Soluble vitamin.It is widely used to the aspects such as medicine, cosmetics, animal feed additive.Because w factor synthetic route is long,
Produce the final products w factor obtaining high-quality, be necessary for the content of intermediate in synthetic route is controlled by.
2,3- dibenzyl succinic acid are a kind of synthetic routes with benzylamine and dibromosuccinic acid as raw material, produced centre
Body, it generates naphthenic acid with triphosgene ring-closure reaction.Due to the particularity insoluble in conventional organic solvent for the 2,3- dibenzyl succinic acid
Matter, current naphthenic acid manufacturing enterprise majority misaligns mesosome 2, and 3- dibenzyl succinic acid carries out content detection control, leads to naphthenic acid to become
Product yield is not high, the low shortcoming of content quality.Only by the content detection to 2,3- dibenzyl succinic acid, could control follow-up
The quality height of product.But, there are no the side with regard to the content detection of 2,3- dibenzyl succinic acid for the open explanation at present
Method.Therefore, present patent application is proposed.
Content of the invention
For the above-mentioned technical problem of prior art, it is an object of the invention to provide a kind of quick detection 2,3- dibenzyl fourth
The method of two acid contents, realizes the detection of the content to 2,3- dibenzyl succinic acid, thus controlling the yield of subsequent reactions product
Height and product quality height.
For reaching above-mentioned purpose, the present invention is achieved by the following technical solutions:
A kind of quick detection 2, the method for 3- dibenzyl succinic acid content, comprise the steps:
(1) step that the scanning of 2,3- dibenzyl succinic acid uv absorption spectra determines maximum absorption wavelength；
(2) preparation process of 2,3- dibenzyl succinic acid standard sample solution；
(3) the acquisition step of 2,3- dibenzyl succinic acid standard curve equation of linear regression；
(4) preparation process of 2,3- dibenzyl succinic acid testing sample；
(5) 2,3- dibenzyl succinic acid ultraviolet detection step；
(6) 2,3- dibenzyl succinic acid concentration calculation procedure.
As preferred, the scanning determination maximum of 2,3- dibenzyl succinic acid uv absorption spectra in described step (1)
The step of absorbing wavelength is as follows: weighs 200mg standard substance 2,3- dibenzyl succinic acid is in 100ml volumetric flask, plus 4.5mg/l
Potassium hydroxide aqueous solution constant volume, then measure 1ml solution with pipet and be diluted to 100ml；Use 1cm quartz colorimetric utensil, with
The potassium hydroxide aqueous solution of 4.5mg/l makees reference, scans in the range of λ is for 190nm-400nm, draws absorption curve, determines λ
Max is 217nm.
As preferred, in described step (2), the preparation process of 2,3- dibenzyl succinic acid standard sample solution is as follows: uses
Deionized water prepares the potassium hydroxide aqueous solution of 4.5mg/l, takes 6 100ml volumetric flasks, uses 4.5mg/l potassium hydroxide water respectively
It is 5 mg/l that solution prepared and diluted becomes concentration, 10 mg/l, 19.76 mg/l, 30.4mg/l, 40.13 mg/l, 50.16 mg/l
2,3- dibenzyl succinic acid standard solution.
As preferred, the acquisition step of 2,3- dibenzyl succinic acid standard curve equation of linear regression in described step (3)
Suddenly as follows: use 1cm quartz colorimetric utensil, with the potassium hydroxide aqueous solution of 4.5mg/l as reference, will be dense for differences multiple in step (2)
The standard sample solution of degree is respectively adopted ultraviolet spectrophotometry and is detected, is 25 DEG C in temperature, humidity is 50% indoor bar
Under part, it is under 217nm in selected wavelength, surveys absorbance, make standard curve；And acquisition mark is calculated according to langbobier law
Directrix curve equation of linear regression.
As preferred, in described step (4), the preparation process of 2,3- dibenzyl succinic acid testing sample is as follows: weighs
300-400mg about workshop testing sample 2,3- dibenzyl succinic acid is in 100ml volumetric flask, plus the hydrogen-oxygen of 4.5mg/l
Change aqueous solutions of potassium constant volume, then measure 1ml solution with pipet and be diluted to 100ml.
As preferred, in described step (5), 2,3- dibenzyl succinic acid ultraviolet detection step is as follows: adopts ultraviolet spectrometry
Absorbance under wavelength is for 217nm for the spectrphotometric method for measuring testing sample.
As preferred, in described step (6), 2,3- dibenzyl succinic acid concentration calculation procedure is as follows: testing sample is existed
Ultraviolet detection wavelength is the measured value of the absorbance under 217nm, substitutes into standard curve equation of linear regression, calculates testing sample
In 2,3- dibenzyl succinic acid concentration, finally content results.
Beneficial effects of the present invention are as follows:
Quick detection 2 of the present invention, the method for 3- dibenzyl succinic acid content, using determined by ultraviolet spectrophotometry 2,3- bis-
Benzyl succinic acid content, the method determination sample 2, the ultraviolet absorption value of 3- dibenzyl succinic acid, then calculating 2,3- dibenzyl
The content of succinic acid, can detection 2 rapidly and efficiently, the content of 3- dibenzyl succinic acid, realize to 2,3- dibenzyl succinic acid
Content detection, thus controlling the yield height of subsequent reactions product and product quality height.The present invention is simple to operate, inspection
Low cost, measurement result accurately it is adaptable in production process intermediate quick mensure.The present invention proposes for the first time in this area
The method of detection 2,3- dibenzyl succinic acid content, is that solid foundation has been established in the development of art technology.
Brief description
Fig. 1 is that the scanning of 2,3- dibenzyl succinic acid uv absorption spectra determines a length of 217nm of maximum absorption wave；
Fig. 2 is the linear relationship chart of 2,3- dibenzyl succinic acid concentration and absorbance in step (3) Plays sample solution.
Specific embodiment
With reference to specific embodiment, the present invention is further illustrated, but protection scope of the present invention is not limited to
This.
Instrument needed for the present invention
The ultraviolet spectrophotometer (tu-1901) buied by Beijing Puxi General Instrument Co., Ltd.
Sample needed for the present invention
2,3- dibenzyl succinic acid standard sample are provided by research and development department of Zhong Xian bio tech ltd of Shangyu city, and 2,3- bis-
6 batches of testing samples of benzyl succinic acid (numbering is 20140601,20140602,20140603,20140604,20140605,
20140606) provided by Zhejiang Sixian Pharmaceutical Co., Ltd.'s naphthenic acid workshop, it is pure that remaining reagent is analysis.
Quick detection 2 of the present invention, the method for 3- dibenzyl succinic acid content, comprise the steps:
(1) step that the scanning of 2,3- dibenzyl succinic acid uv absorption spectra determines maximum absorption wavelength: weigh
200mg standard substance 2,3- dibenzyl succinic acid is in 100ml volumetric flask, plus the potassium hydroxide aqueous solution constant volume of 4.5mg/l, then
Measure 1ml solution with pipet and be diluted to 100ml；Use 1cm quartz colorimetric utensil, make to join with the potassium hydroxide aqueous solution of 4.5mg/l
Ratio scans in the range of λ is for 190nm-400nm, draws absorption curve, determine that λ max is 217nm, as shown in Figure 1:
Instrument performance
INSTRUMENT MODEL: tu-1901
Sequence number: 04-1901-03-0076
Spectral bandwidth: 2.00nm
Spectral scan parameter setting
Sweep limitss: 190.00 to 400.00nm
Luminosity pattern: abs
Sweep spacing: 1.00nm
Scanning speed: fast
Filename: file 6.spd
Creation time: on July 11st, 2014 Friday 9:47:10
Data type: initial data
(2) preparation process of 2,3- dibenzyl succinic acid standard sample solution: deionized water prepares the hydrogen-oxygen of 4.5mg/l
Change aqueous solutions of potassium, take 6 100ml volumetric flasks, becoming concentration with 4.5mg/l potassium hydroxide aqueous solution prepared and diluted respectively is 5 mg/
L, 10 mg/l, 19.76 mg/l, 30.4mg/l, 40.13 mg/l, 50.16 mg/l 2,3- dibenzyl succinic acid standard molten
Liquid.
The acquisition step of (3) 2,3- dibenzyl succinic acid standard curve equation of linear regression: use 1cm quartz colorimetric utensil, with
The potassium hydroxide aqueous solution of 4.5mg/l is reference, and the standard sample solution of multiple variable concentrations in step (2) is respectively adopted purple
Outer spectrophotography is detected, is 25 DEG C in temperature, humidity is under 50% indoor conditionss, is 217nm in selected wavelength
Under, survey absorbance, make standard curve；And acquisition standard curve equation of linear regression, such as Fig. 2 are calculated according to langbobier law
Shown:
Instrument performance
INSTRUMENT MODEL: tu-1901
Sequence number: 04-1901-03-0076
Spectral bandwidth: 2.00nm
Fileinfo
Filename: file 1.qud
Creation time: on July 11st, 2014 Friday 8:03:54
Data type: initial data
Calibration trace
Luminosity pattern: unicast regular way
Curve assessment: no
Curvilinear equation: abs=f(c)
Degree of equation: once
Formula: abs=k1*(c)+k0
Bearing calibration: concentration method
Ko:-0.03991
k1:0.01629
r2:0.9939
Repeated measure: no
Automatic switchover sample cell: no
Quality control:
Zero point is inserted: no
(4) preparation process of 2,3- dibenzyl succinic acid testing sample:
Accurately weigh 2, the 3- dibenzyl succinic acid sample 369.0mg that lot number is 20140601, be placed in 100ml volumetric flask
In, plus the potassium hydroxide aqueous solution constant volume of 4.5mg/l, after shaking up standing, then measure 1ml solution with pipet and be diluted to 100ml.
Accurately weigh 2, the 3- dibenzyl succinic acid sample 374.6mg that lot number is 20140602, be placed in 100ml volumetric flask
In, plus the potassium hydroxide aqueous solution constant volume of 4.5mg/l, after shaking up standing, then measure 1ml solution with pipet and be diluted to 100ml.
Accurately weigh 2, the 3- dibenzyl succinic acid sample 352.2mg that lot number is 20140603, be placed in 100ml volumetric flask
In, plus the potassium hydroxide aqueous solution constant volume of 4.5mg/l, after shaking up standing, then measure 1ml solution with pipet and be diluted to 100ml.
Accurately weigh 2, the 3- dibenzyl succinic acid sample 354.5mg that lot number is 20140604, be placed in 100ml volumetric flask
In, plus the potassium hydroxide aqueous solution constant volume of 4.5mg/l, after shaking up standing, then measure 1ml solution with pipet and be diluted to 100ml.
Accurately weigh 2, the 3- dibenzyl succinic acid sample 364.5mg that lot number is 20140605, be placed in 100ml volumetric flask
In, plus the potassium hydroxide aqueous solution constant volume of 4.5mg/l, after shaking up standing, then measure 1ml solution with pipet and be diluted to 100ml.
Accurately weigh 2, the 3- dibenzyl succinic acid sample 362.9mg that lot number is 20140606, be placed in 100ml volumetric flask
In, plus the potassium hydroxide aqueous solution constant volume of 4.5mg/l, after shaking up standing, then measure 1ml solution with pipet and be diluted to 100ml.
(5) 2,3- dibenzyl succinic acid ultraviolet detection step: with standard curve making the same terms under, using ultraviolet
Absorbance under wavelength is for 217nm for the spectrophotometry testing sample.Measurement result such as table 1.
The measurement result of table 1 testing sample
(6) 2,3- dibenzyl succinic acid concentration calculation procedure.
The absorbance that step (5) is recorded, substitutes into standard curve equation of linear regression, calculates each lot number and treat test sample
The concentration c of product.The 2,3- dibenzyl succinic acid content of sample is c*v/w, and wherein v is to add potassium hydroxide aqueous solution (4.5mg/
L) volume, w is the weight weighing of every batch of testing sample.
Measure the content of the Workshop Production sample of 6 lot numbers as stated above.Result of calculation is as shown in table 2.
Each sample lots result of calculation of table 2
Quick detection 2 of the present invention, the method for 3- dibenzyl succinic acid content, using determined by ultraviolet spectrophotometry 2,3- bis-
Benzyl succinic acid content, the method determination sample 2, the ultraviolet absorption value of 3- dibenzyl succinic acid, then calculating 2,3- dibenzyl
The content of succinic acid, can detection 2 rapidly and efficiently, the content of 3- dibenzyl succinic acid, realize to 2,3- dibenzyl succinic acid
Content detection, thus controlling the yield height of subsequent reactions product and product quality height.The present invention is simple to operate, inspection
Low cost, measurement result accurately it is adaptable in production process intermediate quick mensure.The present invention proposes for the first time in this area
The method of detection 2,3- dibenzyl succinic acid content, is that solid foundation has been established in the development of art technology.
Above-described embodiment is only used for illustrating the inventive concept of the present invention, rather than the restriction to rights protection of the present invention,
All changes that using this design, the present invention is carried out with unsubstantiality, all should fall into protection scope of the present invention.
Claims (6)
1. a kind of quick detection 2, the method for 3- dibenzyl succinic acid content is it is characterised in that comprise the steps:
(1) step that the scanning of 2,3- dibenzyl succinic acid uv absorption spectra determines maximum absorption wavelength；
(2) preparation process of 2,3- dibenzyl succinic acid standard sample solution；
(3) the acquisition step of 2,3- dibenzyl succinic acid standard curve equation of linear regression；
(4) preparation process of 2,3- dibenzyl succinic acid testing sample；
(5) 2,3- dibenzyl succinic acid ultraviolet detection step；
(6) 2,3- dibenzyl succinic acid concentration calculation procedure；
In described step (1), the scanning of 2,3- dibenzyl succinic acid uv absorption spectra determines the step of maximum absorption wavelength such as
Under: weigh 200mg standard substance 2,3- dibenzyl succinic acid is in 100ml volumetric flask, plus the potassium hydroxide aqueous solution of 4.5mg/l
Constant volume, then measure 1ml solution with pipet and be diluted to 100ml；Use 1cm quartz colorimetric utensil, water-soluble with the potassium hydroxide of 4.5mg/l
Liquid makees reference, scans in the range of λ is for 190nm-400nm, draws absorption curve, determines that λ max is 217nm.
2. quick detection 2 as claimed in claim 1, the method for 3- dibenzyl succinic acid content is it is characterised in that described step (2)
The preparation process of middle 2,3- dibenzyl succinic acid standard sample solution is as follows: deionized water prepares the potassium hydroxide of 4.5mg/l
Aqueous solution, takes 6 100ml volumetric flasks, and to become concentration with 4.5mg/l potassium hydroxide aqueous solution prepared and diluted respectively be 5 mg/l, 10
Mg/l, 19.76 mg/l, 30.4mg/l, 40.13 mg/l, the 2,3- dibenzyl succinic acid standard solution of 50.16 mg/l.
3. quick detection 2 as claimed in claim 2, the method for 3- dibenzyl succinic acid content is it is characterised in that described step (3)
In 2,3- dibenzyl succinic acid standard curve equation of linear regression acquisition step as follows: use 1cm quartz colorimetric utensil, with 4.5mg/
The potassium hydroxide aqueous solution of l is reference, and the standard sample solution of multiple variable concentrations in step (2) is respectively adopted ultraviolet spectrometry
Photometry is detected, is 25 DEG C in temperature, humidity is under 50% indoor conditionss, is under 217nm in selected wavelength, surveys and inhale
Luminosity, makes standard curve；And acquisition standard curve equation of linear regression is calculated according to langbobier law.
4. quick detection 2 as claimed in claim 3, the method for 3- dibenzyl succinic acid content is it is characterised in that described step (4)
The preparation process of middle 2,3- dibenzyl succinic acid testing sample is as follows: weigh 300-400mg about workshop testing sample 2,
3- dibenzyl succinic acid is in 100ml volumetric flask, plus the potassium hydroxide aqueous solution constant volume of 4.5mg/l, then measures 1ml with pipet
Solution is diluted to 100ml.
5. quick detection 2 as claimed in claim 4, the method for 3- dibenzyl succinic acid content is it is characterised in that described step (5)
Middle 2,3- dibenzyl succinic acid ultraviolet detection step is as follows: using determined by ultraviolet spectrophotometry testing sample in wavelength is
Absorbance under 217nm.
6. quick detection 2 as claimed in claim 5, the method for 3- dibenzyl succinic acid content is it is characterised in that described step (6)
Middle 2,3- dibenzyl succinic acid concentration calculation procedure is as follows: by absorbance under ultraviolet detection wavelength is for 217nm for the testing sample
Measured value, substitute into standard curve equation of linear regression, calculate the concentration of 2,3- dibenzyl succinic acid in testing sample, finally
Obtain content results.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410428407.4A CN104198423B (en) | 2014-08-28 | 2014-08-28 | Method for rapidly detecting content of 2,3-dibenzyl succinic acid |
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| CN201410428407.4A CN104198423B (en) | 2014-08-28 | 2014-08-28 | Method for rapidly detecting content of 2,3-dibenzyl succinic acid |
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| CN104198423B true CN104198423B (en) | 2017-01-25 |
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5294484A (en) * | 1991-08-03 | 1994-03-15 | Sony Corporation | Polyvinyl aromatic carboxylic acid ester and video printing paper |
| CN102372797A (en) * | 2010-08-12 | 2012-03-14 | 中国石油化工股份有限公司 | Catalyst components for olefin polymerization and catalyst thereof |
-
2014
- 2014-08-28 CN CN201410428407.4A patent/CN104198423B/en not_active Expired - Fee Related
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5294484A (en) * | 1991-08-03 | 1994-03-15 | Sony Corporation | Polyvinyl aromatic carboxylic acid ester and video printing paper |
| CN102372797A (en) * | 2010-08-12 | 2012-03-14 | 中国石油化工股份有限公司 | Catalyst components for olefin polymerization and catalyst thereof |
Non-Patent Citations (1)
| Title |
|---|
| 高效液相色谱法用于米格列奈钙含量和有关物质的研究;宋劲燕 等;《科技情报开发与经济》;20080115;第18卷(第2期);第135-136页 * |
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