CN108982693A - Detection method in relation to substance in a kind of mercaptopropionic acid - Google Patents
Detection method in relation to substance in a kind of mercaptopropionic acid Download PDFInfo
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- CN108982693A CN108982693A CN201810847624.5A CN201810847624A CN108982693A CN 108982693 A CN108982693 A CN 108982693A CN 201810847624 A CN201810847624 A CN 201810847624A CN 108982693 A CN108982693 A CN 108982693A
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/50—Conditioning of the sorbent material or stationary liquid
- G01N30/52—Physical parameters
- G01N30/54—Temperature
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/62—Detectors specially adapted therefor
- G01N30/74—Optical detectors
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N2030/022—Column chromatography characterised by the kind of separation mechanism
- G01N2030/027—Liquid chromatography
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
- G01N2030/062—Preparation extracting sample from raw material
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Abstract
The invention belongs to analytical chemistry fields, and in particular to the detection method in relation to substance in a kind of mercaptopropionic acid, steps are as follows: 1. prepare mercaptopropionic acid product to be tested solution with deionized water；2. first opening UV Absorption detector, it is detected using the ultraviolet light that wavelength is 190 ~ 210nm, then the resulting product to be tested solution of step 1 is injected into the chromatographic column of high performance liquid chromatograph, then gradient elution is carried out with 0.8 ~ 1.0ml/min flow velocity with mobile phase and obtains chromatogram；Each separating degree in relation to substance of mercaptopropionic acid can be calculated according to chromatogram, while the content in relation to substance in mercaptopropionic acid product to be tested is calculated using areas of peak normalization method.Mobile phase used is phosphate aqueous solution-acetonitrile, and the pH of phosphate aqueous solution used is 2.0-3.0；Column temperature is 35~45 DEG C.Method of the invention has the characteristics that blank baseline is noiseless, specificity is strong, separating degree is good, the detection it is suitable for mercaptopropionic acid in relation to substance.
Description
Technical field
The invention belongs to analytical chemistry fields, and in particular to the detection method in relation to substance in a kind of mercaptopropionic acid.
Background technique
The correlation report of detection method currently without mercaptopropionic acid in relation to substance, use mercaptopropionic acid as raw material into
During row chemical reaction, the amount of each impurity has direct influence to subsequent reaction, or even directly affects finished product
The number of middle impurity, but when practical application, in the case where the principal component content of mercaptopropionic acid raw material is essentially identical, different factories
Family, different batches the intermediate or finished product prepared of raw material quality difference it is also bigger, it may be possible to related object therein
Matter content distribution there is caused by biggish difference, but current raw material detection method can not detect it is wherein related
The distribution situation of substance causes raw material effectively be judged and be screened, in order to preferably control the quality of product,
Therefore the detection method of the related substance of mercaptopropionic acid is developed, detection side of the mercaptopropionic acid in relation to substance has finally been determined
Method is screened convenient for the quality to mercaptopropionic acid, so can solve above-mentioned problem.
Summary of the invention
Based on problems of the prior art, the object of the present invention is to provide the inspections in relation to substance in a kind of mercaptopropionic acid
Survey method can be better controlled mercaptopropionic acid quality.
In relation to the detection method of substance in mercaptopropionic acid of the invention, be realized using high performance liquid chromatography, including
Following steps:
(1), ion water making is spent for mercaptopropionic acid product to be tested solution；
(2), UV Absorption detector is first opened, is detected (preferably using the ultraviolet light that wavelength is 190~210nm
Wavelength is 200nm), then the resulting product to be tested solution of step (1) is injected into the chromatographic column of high performance liquid chromatograph, then uses
Mobile phase carries out gradient elution (preferably 0.9ml/min) with 0.7~1.1ml/min flow velocity, obtains the efficient liquid phase of product to be tested
Chromatogram；
The distribution of impurity in mercaptopropionic acid product to be tested can be effectively shown in the present invention according to the chromatogram detected, thus
It may determine that the quality stability of product to be tested, the mercaptopropionic acid raw material for selecting impurity stable is to ensure that the quality of required product is steady
It is qualitative, mercaptopropionic acid and each separating degree in relation to substance can be calculated according to chromatogram in practical applications, while using peak area
Normalization method calculates the content in relation to substance in mercaptopropionic acid product to be tested.
The mobile phase is phosphate aqueous solution-acetonitrile mixture, the pH of the phosphate aqueous solution be 2.0-3.0 (preferably
PH=2.5)；
Column temperature is 35~45 DEG C (preferably 40 DEG C)；
Further, the chromatographic column is using octadecylsilane chemically bonded silica as filler, further, the chromatography
Model Agilent Poroshell 120 EC-C18, internal diameter 4.6mm, length 250mm of column, filler partial size are
2.7μm。
Further, sample volume 1ul.
The gradient elution program are as follows:
Table 1
| Time (minute) | Phosphate aqueous solution (volume %) | Acetonitrile (volume %) |
| 0 | 85 | 15 |
| 15 | 70 | 30 |
| 15.1 | 85 | 15 |
| 19 | 85 | 15 |
In the present invention, term " mercaptopropionic acid " can be the sterling of mercaptopropionic acid, contain in the case where no clearly differentiation
Have mercaptopropionic acid bulk pharmaceutical chemicals or composite, mercaptopropionic acid salt etc. other using mercaptopropionic acid as the product of principal component.This hair
Bright measuring method is suitable for the detection of the said goods, and the measuring method of the related substance of these products is also contained in
In protection scope of the present invention.
In the present invention, term " in relation to substance " refers in the preparation and storage process of mercaptopropionic acid, it is possible to create it is miscellaneous
Matter.
Compared with prior art, the advantages of the present invention are as follows:
Method of the invention has many advantages, such as that blank baseline is noiseless, specificity is strong, separating degree is good, and it is suitable for sulfydryls third
Acid and in the detection in relation to substance, using liquid phase method can it is more intuitive more fully reflection mercaptopropionic acid quality and difference
The specific difference of batch mercaptopropionic acid.
Detailed description of the invention
Fig. 1 is the high-efficient liquid phase chromatogram of blank solution in embodiment 1.
Fig. 2-4 is the high-efficient liquid phase chromatogram of mercaptopropionic acid sample in embodiment 1, and Fig. 2 is that Yuanping City is limited with sharp chemical industry
The chromatogram of the mercaptopropionic acid of responsible company, Fig. 3 are the chromatogram of the mercaptopropionic acid of the far-reaching Chemical Co., Ltd. of Xiaogan, and Fig. 4 is
The chromatogram of the mercaptopropionic acid of lark prestige Science and Technology Ltd..
Fig. 5 is the high-efficient liquid phase chromatogram of mercaptopropionic acid sample in embodiment 2.
Fig. 6 is the high-efficient liquid phase chromatogram of mercaptopropionic acid sample in embodiment 3.
Specific embodiment
Be explained further and illustrate technical solution of the present invention with specific embodiment below, but following embodiment not with
Any mode limits the scope of the invention.
Reagent used in the embodiment of the present invention is bought from the market.
Embodiment 1
(1) testing conditions
Instrument: Thermo U-3000 high performance liquid chromatograph, detector: UV detector, Detection wavelength: 200nm；
Chromatographic column: 120 EC-C18 liquid-phase chromatographic column of Agilent Poroshell (2.7um, 4.6 × 150mm)；
Mobile phase: mobile phase A-Mobile phase B mixed liquor, using pH=2.5 phosphate aqueous solution as mobile phase A, acetonitrile is flowing
Phase B；
Column temperature: 40 DEG C；
Flow velocity: 0.9ml/min；
Sample volume: 1ul；
Linear gradient elution is carried out by the program of table 2.
Table 2
| Time (minute) | Mobile phase A (volume %) | Mobile phase B (volume %) |
| 0 | 85 | 15 |
| 15 | 70 | 30 |
| 15.1 | 85 | 15 |
| 19 | 85 | 15 |
(2) detection method
The preparation of test solution: precision measures mercaptopropionic acid 10ul and is placed in 10ml measuring bottle, is settled to deionized water
Scale shakes up, and as test solution, mercaptopropionic acid used is respectively to be purchased from Yuanping City with the limited duty of sharp chemical industry in the present embodiment
The mercaptopropionic acid sterling of Ren company, the far-reaching Chemical Co., Ltd. of Xiaogan and lark prestige Science and Technology Ltd..
Blank solution: deionized water.
Blank solution and test solution are taken respectively, carry out HPLC analysis according to above-mentioned condition and records chromatogram, as a result
See Fig. 1 (blank solution), Fig. 2 (Yuanping Tongli Chemical Co., Ltd.), Fig. 3 (the far-reaching Chemical Co., Ltd. of Xiaogan) and figure
4 (lark prestige Science and Technology Ltd.s).Each component is respectively 33.03 and 22.43 by appearance sequencing separating degree in Fig. 2, in Fig. 3
Each component by appearance sequencing separating degree is respectively 10.74,22.04,3.17,18.36, in 4.86, Fig. 4 each component by appearance
Sequencing separating degree is respectively 33.26,2.68,23.54, the results showed that, mercaptopropionic acid and its impurity may be implemented in this method
Be kept completely separate, and blank baseline is noiseless, and detection sensitivity is high.
Embodiment 2
It is operated according to the testing conditions and method of embodiment 1, wherein replace with the Detection wavelength of UV detector
190nm, for the mercaptopropionic acid sterling of lark prestige Science and Technology Ltd. as test sample, chromatogram is shown in Fig. 5.
The result shows that this method can realize being kept completely separate for mercaptopropionic acid and its impurity, and blank baseline is noiseless, sensitive
Degree is high.
Embodiment 3
It is operated according to the testing conditions and method of embodiment 1, wherein replace with the Detection wavelength of UV detector
210nm, for the mercaptopropionic acid sterling of lark prestige Science and Technology Ltd. as test sample, chromatogram is shown in Fig. 6.
The result shows that this method can realize being kept completely separate for mercaptopropionic acid and its impurity, and blank baseline is noiseless, sensitive
Degree is high.
Fig. 4's -6 the result shows that, method of the invention can realize being kept completely separate for mercaptopropionic acid and its impurity, and detect
When wavelength 190-210nm, testing result is stablized, and can be efficiently applied to the distribution of detection mercaptopropionic acid impurity.
Claims (8)
1. in relation to the detection method of substance in a kind of mercaptopropionic acid, which is characterized in that the described method comprises the following steps:
1.1 prepare mercaptopropionic acid product to be tested solution with deionized water；
1.2 first open UV Absorption detector, are detected using the ultraviolet light that wavelength is 190~210nm, then by step
1.1 resulting product to be tested solution are injected into the chromatographic column of high performance liquid chromatograph, then with mobile phase with 0.7~1.1ml/min
Flow velocity carries out gradient elution, obtains the high-efficient liquid phase chromatogram of product to be tested；
The mobile phase is phosphate aqueous solution-acetonitrile mixture, and the pH of the phosphate aqueous solution is 2.0-3.0；
Column temperature is 35~45 DEG C.
2. detection method according to claim 1, it is characterised in that: the chromatographic column is with octadecylsilane chemically bonded silica
For filler.
3. detection method according to claim 2, it is characterised in that: the model Agilent of the chromatographic column
Poroshell 120EC-C18, internal diameter 4.6mm, length 250mm, filler partial size are 2.7 μm.
4. detection method according to claim 3, which is characterized in that the program of the gradient elution are as follows:
5. detection method according to claim 4, it is characterised in that: the pH of the phosphate aqueous solution is 2.5.
6. detection method according to claim 5, it is characterised in that: use wavelength in the step 1.2 of the detection method
It is detected for the ultraviolet light of 200nm.
7. detection method according to claim 6, it is characterised in that: sample volume 1ul.
8. detection method according to claim 7, it is characterised in that: the flow velocity of the mobile phase is 0.9ml/min.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201810847624.5A CN108982693A (en) | 2018-07-27 | 2018-07-27 | Detection method in relation to substance in a kind of mercaptopropionic acid |
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| CN201810847624.5A CN108982693A (en) | 2018-07-27 | 2018-07-27 | Detection method in relation to substance in a kind of mercaptopropionic acid |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102575273A (en) * | 2009-04-30 | 2012-07-11 | 三井化学株式会社 | Process for production of 3-mercaptopropionic acid or salt thereof |
| CN104053646A (en) * | 2012-01-27 | 2014-09-17 | 可奥熙搜路司有限公司 | Method for producing 3-mercaptopropionic acid, and carbonic acid ester composition having mercapto group using same, and method for producing thiourethane-based optical materials |
| CN107238664A (en) * | 2017-05-08 | 2017-10-10 | 同济大学苏州研究院 | The method for quantitatively detecting sulfur-containing amino acid in sludge |
-
2018
- 2018-07-27 CN CN201810847624.5A patent/CN108982693A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102575273A (en) * | 2009-04-30 | 2012-07-11 | 三井化学株式会社 | Process for production of 3-mercaptopropionic acid or salt thereof |
| CN104053646A (en) * | 2012-01-27 | 2014-09-17 | 可奥熙搜路司有限公司 | Method for producing 3-mercaptopropionic acid, and carbonic acid ester composition having mercapto group using same, and method for producing thiourethane-based optical materials |
| CN107238664A (en) * | 2017-05-08 | 2017-10-10 | 同济大学苏州研究院 | The method for quantitatively detecting sulfur-containing amino acid in sludge |
Non-Patent Citations (2)
| Title |
|---|
| 周英: "油漆副产物硫化氢合成3-巯基丙酸反应工艺条件", 《中国优秀硕士学位论文全文数据库 工程科技Ⅰ辑》 * |
| 张圣光: "β-巯基丙酸合成工艺研究", 《中国优秀硕士学位论文全文数据库 工程科技Ⅰ辑》 * |
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Address after: 854000 Building 3 of Biomedical Park, Area A, Changdu Economic Development Zone, Tibet Autonomous Region Applicant after: Tibet dorui Pharmaceutical Co., Ltd Address before: 854000 Building 3 of Biomedical Park, Area A, Changdu Economic Development Zone, Tibet Autonomous Region Applicant before: TIBET DUORUI PHARMACEUTICAL Co.,Ltd. |
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Application publication date: 20181211 |