CN109765305A - A kind of efficient liquid phase detection method of 2-chloroethyl amine hydrochloride - Google Patents
A kind of efficient liquid phase detection method of 2-chloroethyl amine hydrochloride Download PDFInfo
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Abstract
Present invention discloses a kind of efficient liquid phase detection methods of 2-chloroethyl amine hydrochloride, firstly, configuring mobile phase by determining chromatographic condition, being filtered, deaerate；Then chromatographic condition is adjusted, chromatographic column is balanced；Configuration standard product solution, test solution and separating degree solution, are injected separately into liquid chromatograph, record respective chromatogram, and the calculating of content, purity and impurity content is carried out according to chromatogram.This method can fast and accurately determine the content of 2-chloroethyl amine hydrochloride, it is ensured that its is quality controllable, reduces error, and easy to operate, appearance time is fast, shortens the detection time in production process, and accuracy is high, substantially increases production efficiency.
Description
Technical field
The present invention relates to a kind of 2-chloroethyl amine hydrochloride efficient liquid phase detection methods, belong to organic analysis technical field.
Background technique
2-chloroethyl amine hydrochloride alias β-chloroethylamine hydrochloride, 2- chloroethyl amine hydrogen chloride, 2 chloroethyl amine hydrochloride etc. are
White is to off-white color flaky crystal.2-chloroethyl amine hydrochloride can carry out many types containing active chlorine atom and active amino
Reaction, be a kind of important chemical products of organic fine containing chlorine, be widely used in medicine, pesticide, table as intermediate
The industries such as face activating agent, dyestuff are also used for the fields such as functional material.According to statistics, 2-chloroethyl amine hydrochloride global supplier more than 120
Family, more than 40 families of domestic vendors, domestic total productive capacity 2000t/a or so, product consumption is every year still with 10% or more speed
Degree increases.
As a kind of important industrial chemicals, 2-chloroethyl amine hydrochloride is also extremely wide in the application of pharmaceuticals industry.2- chlorine
Ethylamine hydrochloride can be used for synthesizing the drugs such as Cefotiam, maleic acid Fu Shaming, taurine, Carmustine.It or amino acid,
The derivative reagent of dipeptide and nucleotide.It is well known that in order to ensure the safety of drug, in pharmaceutical industry in DMF file
Impurity research is an important content.The content of starting material, purity and related impurities are a critically important characteristics.There is no phase
Miscellaneous Quality Research is closed, impurity of also just not knowing where to begin tracking.Unfortunately, although 2-chloroethyl amine hydrochloride industrialized production tens
Year, but the detection of 2-chloroethyl amine hydrochloride also rests on the more original stage.Trace it to its cause may with 2-chloroethyl amine hydrochloride without
Strong functional group absorbs, and polarity is big, is not easy to gasify, and dissociating, it is related to be readily incorporated the properties such as impurity interference.Compare more 2-chloroethyl amines
The COA of hydrochloride supplier, the detection of discovery 2-chloroethyl amine hydrochloride generally only have appearance, dry mistake, fusing point, moisture content, insoluble matter and
Content detection has no and is related to the detection of purity and relative substance, this is not obviously able to satisfy detection of the bulk pharmaceutical chemicals DMF file to raw material
It is required that.2-chloroethyl amine hydrochloride content detection at present is only limitted to titration.Titration detection is to utilize 2-chloroethyl amine hydrochloride
Amido functional group characteristic is detected, and 2-chloroethyl amine hydrochloride synthesis technology needs to use the amino-containing raw material such as ethanol amine,
This causes current titration specificity not good enough.In addition, 2- chloroethene is used in the synthesis of some bulk pharmaceutical chemicals to ensure bulk pharmaceutical chemicals quality
Amine hydrochlorate need to need to carry out the detection in relation to substance chlorethamin in the final product.Above-mentioned titration precision is far from meeting
It is required that specificity is also inadequate.Pharmacopoeia of each country is retrieved and is found, rarely seen TLC method is detected to substance chlorethamin related in bulk pharmaceutical chemicals.
TLC has many advantages, such as micro, quick, simple, but it is a kind of method of quantitative and semi-quantitative, and separating degree also has obvious owe
It lacks, the FDA requirement quantitative to impurity cannot have been met.Meanwhile through detailed investigation of related literatures, do not find that 2-chloroethyl amine hydrochloride is pure temporarily
Degree, the detection method of relative substance etc. also have no the detection method in relation to substance chlorethamin in the bulk pharmaceutical chemicals except TLC.
Summary of the invention
In view of the prior art, there are drawbacks described above, and the purpose of the present invention is to provide a kind of efficient liquid of 2-chloroethyl amine hydrochloride
Phase detection method.
The purpose of the present invention will be realized through the following technical scheme:
A kind of efficient liquid phase detection method of 2-chloroethyl amine hydrochloride, the detection includes containing to 2-chloroethyl amine hydrochloride
Amount, purity and impurity content detection, detect chromatographic condition are as follows:
Instrument: high performance liquid chromatograph prepares UV detector；
Chromatographic column: Agilent Zorbax SB-CN (150mm × 4.6mm, 3.5 μm)；
Mobile phase A: 10mM K2HPO4Aqueous solution (pH=8.0)；
Mobile phase B: CH3CN；
Isocratic elution: mobile phase A: Mobile phase B=40:60；
Detection wavelength: 195nm；
Column temperature: 30 DEG C；
Flow velocity: 0.8mL/min；
Sample volume: 20 μ L；
Dilution: water；
Detecting step is, firstly, configuration mobile phase, is filtered, to deaerate；Then chromatographic condition is adjusted, color is balanced
Compose column；Configuration standard product solution, test solution and separating degree solution, are injected separately into liquid chromatograph, record respective chromatography
Figure carries out the calculating of content, purity and impurity content according to chromatogram.
Preferably, when detecting the content of 2-chloroethyl amine hydrochloride, the standard solution is by dilution to 2- chloroethene
Amine hydrochlorate standard items carry out dissolution constant volume and are made；The test solution is by dilution to 2-chloroethyl amine hydrochloride test sample
Dissolution constant volume is carried out to be made.
Preferably, content passes through external standard method calculating 2-chloroethyl amine hydrochloride when the content detection of the 2-chloroethyl amine hydrochloride
Content.
Preferably, when detecting the purity and impurity content of 2-chloroethyl amine hydrochloride, the contamination levels product solution passes through dilute
Liquid is released to obtained by weighed contamination levels product dissolution constant volume；The separating degree solution is by dilution to weighing 2-chloroethyl amine hydrochloric acid
Salt and contamination levels product carry out obtained by dissolution constant volume；The test solution is by dilution to weighed 2-chloroethyl amine hydrochloride
Obtained by standard items and 2-chloroethyl amine hydrochloride test sample dissolution constant volume, the contamination levels product are ethanol amine.
Preferably, the content of ethanol amine presses the principal component Self-control method of the correction up factor with peak area in the test sample
It calculates, for the content of impurity by principal component Self-control method with calculated by peak area, always miscellaneous is the sum of each impurity in test sample.
Preferably, the percentage of aqueous dibasic potassium phosphate solution and acetonitrile is 40%:60% in the mobile phase；Phosphoric acid hydrogen two
The concentration of aqueous solutions of potassium is 0.01mol/L.
Preferably, the chromatogram column length be 150mm, internal diameter 4.6mm, 3.5 μm of packing material size.
Preferably, the chromatographic column sampling volume of solution is 20 μ L in detection method.
Preferably, the concentration of the standard items and test solution is 1.0mg/mL.
Preferably, the concentration of the 2-chloroethyl amine hydrochloride standard items is 10mg/mL, and the concentration of contamination levels product is 10 μ
g/mL。
What the present invention generated has the technical effect that this method can fast and accurately determine the content of 2-chloroethyl amine hydrochloride,
Ensure that its is quality controllable, reduce error, easy to operate, appearance time is fast, shortens the detection time in production process, accuracy
Height substantially increases production efficiency.
2-chloroethyl amine and ethanol amine raw material peak energy reach good separating effect in this method, can be used for detecting 2- chloroethene
The related substance detection of amine hydrochlorate, and meet bulk pharmaceutical chemicals DMF file to the testing requirements of raw material.
Just attached drawing in conjunction with the embodiments below, the embodiment of the present invention is described in further detail, so that of the invention
Technical solution is more readily understood, grasps.
Detailed description of the invention
Fig. 1: 2-chloroethyl amine hydrochloride content measures corresponding system suitability solution spectrogram in the embodiment of the present invention 1；
Fig. 2: 2-chloroethyl amine hydrochloride content measures corresponding blank solution spectrogram in the embodiment of the present invention 1；
Fig. 3: the corresponding separating degree solution spectrogram of the related substance-measuring of 2-chloroethyl amine hydrochloride in the embodiment of the present invention 3；
Fig. 4: corresponding linear LOQ (10%) solution of the related substance-measuring of 2-chloroethyl amine hydrochloride in the embodiment of the present invention 4
Spectrogram.
Specific embodiment
Method of the invention is illustrated below by specific embodiment, so that technical solution of the present invention is easier to manage
Solution is grasped, but the present invention is not limited thereto.Experimental method described in following embodiments is unless otherwise specified conventional side
Method；The reagent and material commercially obtain unless otherwise specified.
Embodiment 1
The embodiment of the invention provides a kind of efficient liquid phase detection method of 2-chloroethyl amine hydrochloride content, the detection sides
Method content is as follows:
1) chromatographic condition
Instrument: high performance liquid chromatograph prepares UV detector
Chromatographic column: Agilent Zorbax SB-CN (150-mm × 4.6-mm, 3.5- μm)
Mobile phase A: 10mM K2HPO4Aqueous solution (pH=8.0)
Mobile phase B: CH3CN
Isocratic elution: mobile phase A: Mobile phase B=40:60
Detection wavelength: 195nm
Column temperature: 30 DEG C
Flow velocity: 1.0mL/min
Sample volume: 20 μ L
Dilution: water
2) preparation of solution
The preparation of standard solution: it is appropriate that precision weighs 2-chloroethyl amine hydrochloride standard items, is dissolved and is quantified with dilution
Being diluted to concentration is 1.0mg/mL solution.It shakes up, as standard solution.
System suitability solution: i.e. standard solution
It is required that: the RSD of principal component must not be higher than 2.0% in 6 needle system adaptability solution；Tailing factor must not be higher than 1.9.
Test solution: taking 2-chloroethyl amine hydrochloride appropriate, accurately weighed, is dissolved with dilution and is quantitatively diluted to concentration
For the solution of 1.0mg/mL, shake up.Two parts of test solutions are prepared with method.The 2-chloroethyl amine hydrochloride content measurement is corresponding
System suitability solution spectrogram is as shown in Figure 1,2-chloroethyl amine hydrochloride content measures corresponding blank solution spectrogram such as Fig. 2 institute
Show.
3) content calculates:
Its content is calculated with external standard method.
Result=(Ru/Rs) × (Cs/Cu) × Ps × 100
Wherein:
RU: the peak area of 2-chloroethyl amine hydrochloride in test solution；
Cu: the concentration of test sample, mg/mL；
Cs: the concentration of standard items, mg/mL；
PS: the content of standard items, %；
RS: the peak area of standard solution 2-chloroethyl amine hydrochloride.
Embodiment 2
The embodiment of the present invention is the methodological study that efficient liquid phase detects 2-chloroethyl amine hydrochloride content.Chromatographic condition is the same as real
Apply example 1.
1) system suitability is tested
Accurate 6 parts of solution of extraction system adaptability respectively, is operated by method, is injected separately into liquid chromatograph, records chromatography
Figure, while doing blank test.Investigate the RSD (%) of the peak area of principal component.
System suitability result see the table below；
There is the RSD of 6 needle peak areas known to table less than 2%, tailing factor is lower than 1.9, liquid content inspection provided by the invention
It is good to survey method system applicability.
2) specificity
Blank solution, standard solution and each portion of test solution are taken, liquid chromatograph is injected, chromatogram is recorded, examines
Whether the retention time for examining component in test solution is consistent with standard solution.
| Sample | STD | TS |
| RT(min) | 3.422 | 3.450 |
3) linear and range
Precision weighs 2-chloroethyl amine hydrochloride working standard 100mg, sets in 10mL volumetric flask, dilution is dissolved and diluted
To scale, shake up；Precision measures stock solution 0.8mL, 0.9mL, 1.0mL, 1.1mL and 1.2mL and splits in 10mL measuring bottle, with dilution
Liquid is diluted to scale, shakes up, as the test solution of linear test, takes 20 μ L of solution respectively, injects liquid chromatograph, records color
Spectrogram.As a result it counts as follows:
With the function construction of 2-chloroethyl amine hydrochloride peak area and concentration, then with least-squares linear regression, standard is obtained
Curvilinear equation are as follows: y=8423x-36.81 calculates correlation coefficient r2=0.9997.Analysis method is linearly good.
4) rate of recovery
Precision weighs 2-chloroethyl amine hydrochloride working standard 200.0mg and sets in 20mL measuring bottle, add dilution dissolve and it is dilute
It releases to scale, as standard items stock solution；Take 9 10mL volumetric flasks label 1~9 respectively, precision in 1~No. 3 volumetric flask
0.8mL standard items stock solution, accurate addition 1mL standard items stock solution in 4~No. 6 volumetric flasks, 7~No. 9 volumetric flasks are added
Middle accurate addition 1.2mL standard items stock solution, adds diluted to scale, 20 μ L is then taken to inject liquid chromatograph, note
Record chromatogram.Test result is as follows:
As can be seen from the above table, the rate of recovery of 2-chloroethyl amine hydrochloride is between 98.0%~102.0%, 9 parts of RSD value
It is 1.4%.Rate of recovery result is good.
5) durability (stability of solution)
Prepare test solution and standard solution, then at room temperature, by volumetric flask standard solution and
Test solution places 0h, for 24 hours, after 48h, injects liquid chromatograph, records chromatogram.It is examined with the standard solution of Fresh
Examine the variation of its testing result.
Test result is as follows table:
By table it can be concluded that the RSD of main peak content is 0.2% in standard solution, main peak content in test solution
RSD is 0.5%；Test solution and standard solution provided by the invention are placed at room temperature for 48h and have good stability.
Embodiment 3
The embodiment of the present invention provides a kind of efficient liquid phase detection method of the 2-chloroethyl amine hydrochloride in relation to substance, the detection
Method content is as follows:
1) chromatographic condition: with embodiment 1.
2) preparation of solution:
Separating degree solution: precision weighs 2-chloroethyl amine hydrochloride and appropriate ethanol amine, is dissolved with dilution and quantifies dilution
It is respectively the mixed solution of 10.0 μ g/mL and 50.0 μ g/mL at concentration.It shakes up, as separating degree solution.
Contamination levels product solution: it is appropriate that precision weighs 2-chloroethyl amine hydrochloride, is dissolved and is quantitatively diluted to dense with dilution
Degree is respectively the solution of 10.0 μ g/mL.It shakes up, as contamination levels product solution.
It is required that: the RSD of principal component must not be higher than 5.0% in 6 needle contamination levels product solution；2-chloroethyl amine in separating degree solution
Hydrochloride and ethanol amine separating degree must not be lower than 2.0.
Test solution: taking test sample appropriate, accurately weighed, is dissolved with dilution and is quantitatively diluted to concentration and is
The solution of 10.0mg/mL, shakes up.Two parts of test solutions are prepared with method.
Ethanol amine: its content is calculated with the principal component Self-control method of the correction up factor；
Unknown impuritie: its content is calculated with principal component Self-control method；Total impurities are the sum of each impurity.
3) related content of material calculates
The calculating of ethanol amine:
Result=(Ru/Rs)×(Cs/Cu)×Ps×CF×100
Wherein:
RU: the peak area of ethanol amine in test solution；
Cs: the concentration of contamination levels product solution 2-chloroethyl amine hydrochloride, mg/mL；
Cu: the concentration of test solution, mg/mL；
RS: the peak area of contamination levels product solution 2-chloroethyl amine hydrochloride；
PS: the content of 2-chloroethyl amine hydrochloride standard items, %；
CF: correction factor
The calculating of unknown impuritie:
Result=(Ru/Rs)×(Cs/Cu)×Ps×100
Wherein:
RU: the peak area of unknown impuritie in test solution；
Cs: the concentration of contamination levels product solution 2-chloroethyl amine hydrochloride, mg/mL；
Cu: the concentration of test solution, mg/mL；
RS: the peak area of contamination levels product solution 2-chloroethyl amine hydrochloride；
PS: the content of 2-chloroethyl amine hydrochloride standard items, %.
The corresponding separating degree solution spectrogram of the related substance-measuring of above 2-chloroethyl amine hydrochloride is as shown in Figure 3.
Embodiment 4
The embodiment of the present invention is that efficient liquid phase detects methodological study of the 2-chloroethyl amine hydrochloride in relation to substance.Chromatographic condition
With embodiment 1.
1) system suitability is tested
It accurate 6 parts and 1 part of separating degree solution of extraction system adaptability solution respectively, is operated by method, is injected separately into liquid phase
Chromatograph records chromatogram, while doing blank test.Investigate the RSD of the peak area of the separating degree and principal component between each component
(%).
System suitability result see the table below:
Less than 2%, the separating degree between main composition and ethanol amine is greater than the RSD of the main composition peak area of 6 needles as seen from table
2.0, liquid content detection method system suitability provided by the invention is good.
2) specificity
Blank solution, standard solution and each portion of test solution are taken, liquid chromatograph is injected, chromatogram is recorded, examines
Whether the retention time for examining component in test solution is consistent with standard solution.
| Sample | Position solution-ethanol amine | TS |
| RT(min) | 6.798 | 6.644 |
3) quantitative limit and detection limit
Precision weighs 2-chloroethyl amine hydrochloride and appropriate ethanol amine, with diluted until reaching 2-chloroethyl amine hydrochloride
Detection with ethanol amine limits (LOD) and quantitative limit (LOQ), 2-chloroethyl amine hydrochloride and ethanolamine concentration is calculated, as detection
Limit and quantitative limit solution.It takes detection limit solution a, injects liquid chromatograph, record chromatogram.Six parts of quantitative limit solution are taken, note
Enter liquid chromatograph, records chromatogram.
4) linear and range
Precision weighs 2-chloroethyl amine hydrochloride and ethanol amine working standard each 12.5mg and 62.5mg, sets 50mL measuring bottle
In, dilution dissolves and is diluted to scale, shakes up, as linear stock solution；The linear stock solution 0.1mL of precision measurement,
0.2mL, 0.5mL, 0.8mL, 1.0mL and 1.5mL are split in 25mL measuring bottle, with diluted to scale, are shaken up, as linearly
Solution takes 20 μ L of linear solvent respectively, injects liquid chromatograph, records chromatogram.As a result it counts as follows:
With the function construction of peak area and concentration, then with least-squares linear regression, calibration curve equation is obtained, calculate phase
Relationship number r2.Calculate the calibration curve equation of final result 2-chloroethyl amine hydrochloride are as follows: y=5.8764x-1.4946, r2=
0.999.The calibration curve equation of ethanol amine are as follows: y=5.7514x+0.1413, r2=0.9999.Analysis method is linearly good.2-
Corresponding linear LOQ (10%) the solution spectrogram of the related substance-measuring of chloroethylamine hydrochloride is as shown in Figure 4.
5) rate of recovery
The test sample 2.5g that precision weighs known exact level is set in 10mL volumetric flask, is added dilution to dissolve and is diluted to quarter
Degree, as test sample stock solution；Another precision weighs that ethanol amine working standard is appropriate, and it is respectively 1.25mg/mL that concentration, which is made,
Mixed solution, as contamination levels product stock solution 1；Another precision pipettes contamination levels product stock solution 1 in 10mL volumetric flask
In, add dilution to dissolve and be diluted to scale, as contamination levels product stock solution 2, takes 9 25mL volumetric flasks label 1 respectively
~No. 9, in 1~No. 3 volumetric flask it is accurate be added 1.0mL test sample stock solution and 1.0mL contamination levels product stock solution 2,4~
It is accurate in No. 6 volumetric flasks that 1,7~No. 9 volumetric flasks of 1.0mL test sample stock solution and 1.0mL contamination levels product stock solution are added
It is middle it is accurate 1.0mL test sample stock solution and 2.0mL contamination levels product stock solution 1 is added, add diluted to scale, so
After take 20 μ L inject liquid chromatograph, record chromatogram.
Test result is as follows:
As can be seen from the above table, between 80.0%~120.0%, 9 parts of RSD value should be lower than the rate of recovery of ethanol amine
15.0%.Rate of recovery result is good.
6) durability (stability of solution)
Prepare test solution and standard solution, then at room temperature, by volumetric flask standard solution and
Test solution places 0h, for 24 hours, after 48h, injects liquid chromatograph, records chromatogram.It is examined with the standard solution of Fresh
Examine the variation of its testing result.
Test result is as follows table:
By table it can be concluded that testing result has no significant change after test solution and standard solution place 48h.
Test solution and standard solution provided by the invention are placed at room temperature for 48h and have good stability.
Still there are many specific embodiments by the present invention.All all skills formed using equivalent replacement or equivalent transformation
Art scheme, all falls within the scope of protection of present invention.
Claims (10)
1. a kind of efficient liquid phase detection method of 2-chloroethyl amine hydrochloride, it is characterised in that: the detection includes to 2-chloroethyl amine
Content, purity and the impurity content detection of hydrochloride, detect chromatographic condition are as follows:
Instrument: high performance liquid chromatograph prepares UV detector；
Chromatographic column: Agilent Zorbax SB-CN(150 mm × 4.6mm, 3.5 μm)；
Mobile phase A: 10 mM K2HPO4Aqueous solution (pH=8.0)；
Mobile phase B: CH3CN；
Isocratic elution: mobile phase A: Mobile phase B=40:60；
Detection wavelength: 195 nm；
Column temperature: 30 DEG C；
Flow velocity: 0.8 mL/min；
Sample volume: 20 μ L；
Dilution: water；
Detecting step is, firstly, configuration mobile phase, is filtered, to deaerate；Then chromatographic condition is adjusted, chromatographic column is balanced；
Configuration standard product solution, test solution and separating degree solution, are injected separately into liquid chromatograph, record respective chromatogram, root
The calculating of content, purity and impurity content is carried out according to chromatogram.
2. a kind of efficient liquid phase detection method of 2-chloroethyl amine hydrochloride according to claim 1, it is characterised in that: work as inspection
When surveying the content of 2-chloroethyl amine hydrochloride, the standard solution carries out 2-chloroethyl amine hydrochloride standard items by dilution molten
Constant volume is solved to be made；The test solution carries out dissolution constant volume to 2-chloroethyl amine hydrochloride test sample by dilution and is made.
3. a kind of efficient liquid phase detection method of 2-chloroethyl amine hydrochloride according to claim 2, it is characterised in that: described
Content calculates the content of 2-chloroethyl amine hydrochloride by external standard method when the content detection of 2-chloroethyl amine hydrochloride.
4. a kind of efficient liquid phase detection method of 2-chloroethyl amine hydrochloride according to claim 1, it is characterised in that: work as inspection
When surveying the purity and impurity content of 2-chloroethyl amine hydrochloride, the contamination levels product solution is by dilution to weighed impurity mark
Obtained by quasi- product dissolution constant volume；The separating degree solution is carried out by dilution to 2-chloroethyl amine hydrochloride and contamination levels product are weighed
It dissolves obtained by constant volume；The test solution is by dilution to weighed 2-chloroethyl amine hydrochloride standard items and 2-chloroethyl amine salt
Hydrochlorate test sample dissolves obtained by constant volume, and the contamination levels product are ethanol amine.
5. a kind of efficient liquid phase detection method of 2-chloroethyl amine hydrochloride according to claim 4, it is characterised in that: described
In test sample the content of ethanol amine by the principal component Self-control method of the correction up factor with calculated by peak area, impurity in test sample
For content by principal component Self-control method with calculated by peak area, always miscellaneous is the sum of each impurity.
6. a kind of efficient liquid phase detection method of 2-chloroethyl amine hydrochloride according to claim 1, it is characterised in that: described
The percentage of aqueous dibasic potassium phosphate solution and acetonitrile is 40%:60% in mobile phase；The concentration of aqueous dibasic potassium phosphate solution is
0.01mol/L。
7. a kind of efficient liquid phase detection method of 2-chloroethyl amine hydrochloride according to claim 1, it is characterised in that: described
Chromatogram column length is 150mm, internal diameter 4.6mm, 3.5 μm of packing material size.
8. a kind of efficient liquid phase detection method of 2-chloroethyl amine hydrochloride according to claim 1, it is characterised in that: detection
The chromatographic column sampling volume of solution is 20 μ L in method.
9. a kind of efficient liquid phase detection method of 2-chloroethyl amine hydrochloride according to claim 2, it is characterised in that: described
The concentration of standard items and test solution is 1.0mg/mL.
10. a kind of efficient liquid phase detection method of 2-chloroethyl amine hydrochloride according to claim 4, it is characterised in that: institute
The concentration for stating 2-chloroethyl amine hydrochloride standard items is 10mg/mL, and the concentration of contamination levels product is 10 μ g/mL.
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2721419B2 (en) * | 1990-09-11 | 1998-03-04 | 三井東圧化学株式会社 | Method for producing mercaptoamines |
| CN108129260A (en) * | 2017-12-21 | 2018-06-08 | 常州南京大学高新技术研究院 | A kind of synthetic method of styrene glycol |
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2018
- 2018-12-13 CN CN201811523455.6A patent/CN109765305B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2721419B2 (en) * | 1990-09-11 | 1998-03-04 | 三井東圧化学株式会社 | Method for producing mercaptoamines |
| CN108129260A (en) * | 2017-12-21 | 2018-06-08 | 常州南京大学高新技术研究院 | A kind of synthetic method of styrene glycol |
Non-Patent Citations (2)
| Title |
|---|
| MICHAL DOUŠA等: "HILIC–MS Determination of Genotoxic Impurity of 2-Chloro-N-(2-Chloroethyl)Ethanamine in the Vortioxetine Manufacturing Process", 《JOURNAL OF CHROMATOGRAPHIC SCIENCE》 * |
| TOJIO TSUSHIDA等: "高效液相色谱法测定茶新梢和成茶中的乙胺含量", 《茶叶》 * |
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