CN113156003A - Method for detecting tert-butylamine in arotinolol hydrochloride - Google Patents
Method for detecting tert-butylamine in arotinolol hydrochloride Download PDFInfo
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- CN113156003A CN113156003A CN202110358235.8A CN202110358235A CN113156003A CN 113156003 A CN113156003 A CN 113156003A CN 202110358235 A CN202110358235 A CN 202110358235A CN 113156003 A CN113156003 A CN 113156003A
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- butylamine
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- YBRBMKDOPFTVDT-UHFFFAOYSA-N tert-butylamine Chemical compound CC(C)(C)N YBRBMKDOPFTVDT-UHFFFAOYSA-N 0.000 title claims abstract description 26
- BHIAIPWSVYSKJS-UHFFFAOYSA-N arotinolol Chemical compound S1C(SCC(O)CNC(C)(C)C)=NC(C=2SC(=CC=2)C(N)=O)=C1 BHIAIPWSVYSKJS-UHFFFAOYSA-N 0.000 title claims abstract description 23
- 229950010731 arotinolol Drugs 0.000 title claims abstract description 23
- 238000000034 method Methods 0.000 title claims abstract description 15
- 239000001257 hydrogen Substances 0.000 claims abstract description 8
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 8
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 5
- 125000004435 hydrogen atom Chemical group [H]* 0.000 claims abstract description 3
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 51
- WQDUMFSSJAZKTM-UHFFFAOYSA-N Sodium methoxide Chemical compound [Na+].[O-]C WQDUMFSSJAZKTM-UHFFFAOYSA-N 0.000 claims description 28
- 239000000523 sample Substances 0.000 claims description 12
- 238000001514 detection method Methods 0.000 claims description 11
- 238000005303 weighing Methods 0.000 claims description 10
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 6
- 239000012488 sample solution Substances 0.000 claims description 4
- 150000001412 amines Chemical class 0.000 claims description 3
- 239000012159 carrier gas Substances 0.000 claims description 3
- 229910052757 nitrogen Inorganic materials 0.000 claims description 3
- 239000002904 solvent Substances 0.000 claims description 3
- 239000003513 alkali Substances 0.000 claims description 2
- 238000004587 chromatography analysis Methods 0.000 claims 2
- 239000000243 solution Substances 0.000 abstract description 17
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 abstract description 8
- 238000004817 gas chromatography Methods 0.000 abstract description 4
- 238000002360 preparation method Methods 0.000 abstract description 4
- 230000035945 sensitivity Effects 0.000 abstract description 3
- 239000012085 test solution Substances 0.000 abstract description 3
- 238000012795 verification Methods 0.000 abstract description 2
- 238000011084 recovery Methods 0.000 description 6
- 239000011550 stock solution Substances 0.000 description 6
- 239000002876 beta blocker Substances 0.000 description 2
- 229940097320 beta blocking agent Drugs 0.000 description 2
- 239000003814 drug Substances 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 239000012088 reference solution Substances 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- 206010002383 Angina Pectoris Diseases 0.000 description 1
- 208000007530 Essential hypertension Diseases 0.000 description 1
- 208000001871 Tachycardia Diseases 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 206010003119 arrhythmia Diseases 0.000 description 1
- 230000006793 arrhythmia Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 239000012153 distilled water Substances 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 201000006517 essential tremor Diseases 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 230000009965 odorless effect Effects 0.000 description 1
- 238000005220 pharmaceutical analysis Methods 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000012916 structural analysis Methods 0.000 description 1
- 230000006794 tachycardia Effects 0.000 description 1
- 230000009967 tasteless effect Effects 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
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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
-
- 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
- G01N30/14—Preparation by elimination of some components
-
- 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
- G01N30/16—Injection
-
- 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
- G01N30/26—Conditioning of the fluid carrier; Flow patterns
- G01N30/28—Control of physical parameters of the fluid carrier
- G01N30/30—Control of physical parameters of the fluid carrier of temperature
-
- 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
- G01N30/26—Conditioning of the fluid carrier; Flow patterns
- G01N30/28—Control of physical parameters of the fluid carrier
- G01N30/32—Control of physical parameters of the fluid carrier of pressure or speed
-
- G01N30/482—
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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
- G01N30/64—Electrical detectors
- G01N30/68—Flame ionisation detectors
-
- 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
- G01N30/26—Conditioning of the fluid carrier; Flow patterns
- G01N30/28—Control of physical parameters of the fluid carrier
- G01N30/32—Control of physical parameters of the fluid carrier of pressure or speed
- G01N2030/324—Control of physical parameters of the fluid carrier of pressure or speed speed, flow rate
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- G01N2030/484—
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- General Health & Medical Sciences (AREA)
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- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
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Abstract
The invention discloses a method for detecting tert-butylamine in arotinolol hydrochloride, which is a gas chromatography and is provided with a hydrogen flame ionization detector, wherein the detector is a hydrogen flame ionization detector (FID for short), the temperature is 248-252 ℃, and 250 ℃ is optimally selected; the temperature of a sample inlet is 148-152 ℃, and 150 ℃ is optimally selected; the flow rate of the chromatographic column is 0.9-1.1ml/min, and 1.0ml/min is optimally selected; the temperature raising program of the chromatographic column is that the initial temperature is 60 ℃, the temperature is maintained for 13min, and then the temperature is raised to 240 ℃ at the speed of 30 ℃/min and maintained for 10 min; directly injecting sample with the volume of 1 mul; the split ratio is 10:1, and the preparation of the test solution: 0.5g of arotinolol hydrochloride was weighed out. After the arotinolol hydrochloride is dissolved, the solution contains free hydrochloric acid reaction, so that the tert-butylamine cannot be detected. The method carries out complete verification and has the advantages of high sensitivity, good specificity, simple operation and the like.
Description
Technical Field
The invention relates to a method for detecting tert-butylamine in arotinolol hydrochloride in the field of pharmaceutical analysis
Background
Arotinolol hydrochloride is white powder, odorless and tasteless.
Arotinolol hydrochloride, known as the fourth generation beta blocker, is the first line drug of beta blockers. The traditional Chinese medicine composition is mainly used for treating mild to moderate essential hypertension, angina, tachycardia arrhythmia and essential tremor.
The examination item of the tert-butylamine in the arotinolol hydrochloride is not determined under the item of the varieties of arotinolol hydrochloride in 'Chinese pharmacopoeia' 2020 edition, and the detection of the tert-butylamine in the arotinolol hydrochloride is not collected in the pharmacopoeias such as United states pharmacopoeia, European pharmacopoeia and the like which can be searched. No report is found about the detection of tert-butylamine in arotinolol hydrochloride.
As can be seen from the structural analysis of the arotinolol hydrochloride, the hydrochloric acid exists in the molecular structure, so that the sample solution is considered to contain free hydrochloric acid to react with the tert-butylamine, and the tert-butylamine cannot be detected; therefore, the detection method can be established by considering that a proper amount of alkali solution is added and accurately detecting the tert-butylamine on the premise of not introducing new impurities.
According to the above analysis, a sodium methoxide solution was added during the dissolution of the sample, thereby performing a complete set of method verification, including: specificity, detection and quantitation limits, linearity and range, accuracy, precision, solution stability, durability.
Disclosure of Invention
Technical problem to be solved
The invention provides a method for detecting tert-butylamine in arotinolol hydrochloride, which adopts gas chromatography for detection and has the advantages of high sensitivity, good accuracy and easy operation.
(II) technical scheme
The invention discloses a method for detecting tert-butylamine in arotinolol hydrochloride, which is a gas chromatography and is provided with a hydrogen flame ionization detector (FID for short). After the arotinolol hydrochloride is dissolved, the solution contains free hydrochloric acid reaction, so that the tert-butylamine cannot be detected.
The detector is a hydrogen flame ionization detector (FID for short), the temperature is 248-252 ℃, and 250 ℃ is optimally selected; the temperature of a sample inlet is 148-152 ℃, and 150 ℃ is optimally selected; the flow rate of the chromatographic column is 0.9-1.1ml/min, and 1.0ml/min is optimally selected; the temperature raising program of the chromatographic column is that the initial temperature is 60 ℃, the temperature is maintained for 13min, and then the temperature is raised to 240 ℃ at the speed of 30 ℃/min and maintained for 10 min; directly injecting sample with the volume of 1 mul; the split ratio was 10: 1.
The method comprises the following steps:
(1) preparation of a test solution: weighing 0.5g arotinolol hydrochloride, placing in a 10ml volumetric flask, adding a small amount of methanol, accurately adding sodium methoxide solution (weighing 2.4g of sodium methoxide, placing in a 50ml volumetric flask, metering the volume to the scale with methanol, mixing uniformly) by 5ml, shaking violently until the sample is completely dissolved, metering the volume to the scale with methanol, mixing uniformly, and preparing into a sample solution with the concentration of 50 mg/ml.
(2) Preparation of control solutions: weighing 16mg of tert-butylamine, putting the tert-butylamine in a 50ml volumetric flask, fixing the volume by using methanol, precisely weighing 1ml of comparison stock solution, putting the comparison stock solution in a 20ml volumetric flask, and fixing the volume by using the methanol to prepare a comparison solution with the concentration of 16 mu g/ml.
(III) advantageous effects
Compared with the prior art, the method for detecting the tert-butylamine in the arotinolol hydrochloride has the following beneficial effects:
the method for detecting the tert-butylamine in the arotinolol hydrochloride is a gas chromatography method and is characterized by adopting an amine-based column, a hydrogen flame ionization detector (FID for short), taking nitrogen as a carrier gas, adding a proper amount of sodium methoxide into methanol as a solvent, and directly injecting a sample. Has the advantages of high efficiency and sensitivity, and can be widely applied to the detection of the tert-butylamine in the arotinolol hydrochloride.
Drawings
FIG. 1 is a map of the applicability of the system of the present invention;
FIG. 2 is a table of peaks of applicability of the system of the present invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example one
Chromatographic conditions are as follows: a chromatographic column: InertCap for Amines, 0.32 mm. times.30 m.
Column temperature: the initial temperature is 60 ℃, the temperature is maintained for 13min, and then the temperature is increased to 240 ℃ at the speed of 30 ℃/min, and the temperature is maintained for 10 min.
Detector temperature: at 250 ℃ to obtain a mixture.
Sample inlet temperature: at 150 ℃.
Carrier gas: high purity nitrogen.
Flow rate: 1 ml/min; hydrogen flow rate: 40 ml/min; air flow rate: 400 ml/min.
The split ratio is as follows: 10:1.
Sample introduction amount: 1 μ l.
Preparation of solutions
Sodium methoxide solution: weighing 2.4g of sodium methoxide, putting the sodium methoxide into a 50ml volumetric flask, metering the volume to a scale with methanol, and uniformly mixing;
preparing a control solution:
weighing 16mg of tert-butylamine, putting the tert-butylamine in a 50ml volumetric flask, and fixing the volume by using methanol; precisely measuring 1ml from the medium, placing the solution in a 20ml volumetric flask, and performing constant volume with methanol to obtain a reference solution; the concentration was 16. mu.g/ml.
Precisely measuring 1 μ l of the reference solution, injecting into a gas chromatograph, recording chromatogram, and obtaining baseline separation between main components and impurities with separation degree of 1.5 or more as shown in figure 1.
Example two
Recovery control stock solution: precisely weighing 16mg of tert-butylamine into a 50ml volumetric flask, dissolving with methanol, and fixing the volume to prepare the tert-butylamine with the concentration of 320 mu g/ml; recovery was compared to the stock solution.
Recovery control solution: the yield control stock solution was taken back in 1ml to 20ml volumetric flasks and the volume was determined by adding methanol.
Test solution: taking about 500mg of arotinolol hydrochloride, precisely weighing, adding distilled water to dissolve and dilute to 10ml, and preparing a sample solution with the concentration of 5 mg/ml.
Accuracy solution: taking 500mg of each sample, precisely weighing the samples into a 10ml volumetric flask, adding 5ml of sodium methoxide solution to completely dissolve the samples, then adding control solutions according to the limited 80%, 100% and 120%, namely adding recovery rate control stock solutions of 0.4ml, 0.5ml and 0.6ml respectively, adding methanol to dissolve and fixing the volume.
Percent recovery ═ (measured-as-received)/added 100%.
The average recovery rate of the tert-butylamine is between 80 and 120 percent.
Claims (7)
1. A method for detecting tert-butylamine in arotinolol hydrochloride is characterized by adopting an amine-based column, a hydrogen flame ionization detector, nitrogen as a carrier gas, methanol and a proper amount of sodium methoxide as a solvent, and directly injecting a sample.
2. The detection method according to claim 1, wherein the sample is dissolved in a solvent and an added alkali solution is methanol or sodium methoxide.
3. The detection method according to claims 1-2, wherein the flow rate of the chromatography column is 0.9-1.1ml/min, and the flow rate of the chromatography column is 1.0 ml/min.
4. A method of detection as claimed in claims 1 to 3 wherein the detector temperature is 248 to 252 ℃ and the detector temperature is 250 ℃.
5. The detection method according to claim 1, wherein the inlet temperature is 148 to 152 ℃ and the inlet temperature is 150 ℃.
6. The detection method according to claim 1, wherein the initial temperature is 58 to 62 ℃ and the initial temperature is 60 ℃.
7. The method of claim 1, further comprising the steps of:
(1) preparing arotinolol hydrochloride into a sample solution with the concentration of 50mg/ml by using a sodium methoxide solution; preparing a control solution with the concentration of 16 mu g/ml from tert-butylamine, wherein the methanol solution comprises the following steps: weighing 2.4g of sodium methoxide, putting the sodium methoxide into a 100ml volumetric flask, metering the volume to the scale with methanol, and mixing the sodium methoxide and the methanol uniformly.
The detector is a hydrogen flame ionization detector, the temperature is 248-252 ℃, and 250 ℃ is optimally selected; the temperature of a sample inlet is 148-152 ℃, and 150 ℃ is optimally selected; the flow rate of the chromatographic column is 0.9-1.1ml/min, and 1.0ml/min is optimally selected; the temperature raising program of the chromatographic column is that the initial temperature is 60 ℃, the temperature is maintained for 13min, and then the temperature is raised to 240 ℃ at the speed of 30 ℃/min and maintained for 10 min; directly injecting sample with the volume of 1 mul; the split ratio was 10: 1.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110358235.8A CN113156003A (en) | 2021-04-01 | 2021-04-01 | Method for detecting tert-butylamine in arotinolol hydrochloride |
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| Application Number | Priority Date | Filing Date | Title |
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| CN202110358235.8A CN113156003A (en) | 2021-04-01 | 2021-04-01 | Method for detecting tert-butylamine in arotinolol hydrochloride |
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103626750A (en) * | 2013-11-15 | 2014-03-12 | 北京博爱旺康医药科技有限公司 | High-purity arotinolol hydrochloride and preparation method thereof |
| CN108026048A (en) * | 2015-09-11 | 2018-05-11 | 东丽株式会社 | The manufacture method of epsilon-caprolactams |
| CN108226338A (en) * | 2017-12-29 | 2018-06-29 | 天津红日药业股份有限公司 | One kind contains sarpogrelate hydrochloride intermediate dimethylamine detection method |
| CN111289676A (en) * | 2020-01-20 | 2020-06-16 | 南京林业大学 | Method for detecting residual tert-butylamine in terbutaline sulfate bulk drug |
| CN111650289A (en) * | 2020-04-16 | 2020-09-11 | 江苏艾立康药业股份有限公司 | Method for determining related substances of 3-chloro-1- (N, N-dimethyl) propylamine hydrochloride |
-
2021
- 2021-04-01 CN CN202110358235.8A patent/CN113156003A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103626750A (en) * | 2013-11-15 | 2014-03-12 | 北京博爱旺康医药科技有限公司 | High-purity arotinolol hydrochloride and preparation method thereof |
| CN108026048A (en) * | 2015-09-11 | 2018-05-11 | 东丽株式会社 | The manufacture method of epsilon-caprolactams |
| CN108226338A (en) * | 2017-12-29 | 2018-06-29 | 天津红日药业股份有限公司 | One kind contains sarpogrelate hydrochloride intermediate dimethylamine detection method |
| CN111289676A (en) * | 2020-01-20 | 2020-06-16 | 南京林业大学 | Method for detecting residual tert-butylamine in terbutaline sulfate bulk drug |
| CN111650289A (en) * | 2020-04-16 | 2020-09-11 | 江苏艾立康药业股份有限公司 | Method for determining related substances of 3-chloro-1- (N, N-dimethyl) propylamine hydrochloride |
Non-Patent Citations (2)
| Title |
|---|
| M.MOHNKE等: "Application of a fused-silica column to the determination of very volatile amines by gas-solid chromatography", 《JOURNAL OF CHROMATOGRAPHY A》 * |
| 胡晓明等: "气相色谱法测定叔丁胺及有机杂质含量", 《分析与测试》 * |
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