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Detection method of impurities in 3-amino-2-butenoic acid methyl ester

A technology of methyl crotonate and detection method, applied in the directions of measuring devices, instruments, scientific instruments, etc., can solve the problems such as affecting the drug effect of preparation nitrendipine tablets, not being found, affecting the quality and the like

Active Publication Date: 2020-07-07
湖南新领航检测技术有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0002] The English name of 3-amino-2-butenoic acid methyl ester is Methyl 3-aminocrotonate, also known as β-aminocrotonate methyl ester, and its molecular formula is C 5 h 9 NO 2 , molecular weight is 115.13, chemical structure formula: 3-Amino-2-butenoic acid methyl ester is the starting material of the raw material drug nitrendipine, and the literature that can be consulted at present shows that the synthesis of the nitrendipine raw material drug uses 3-amino-2-butenoic acid methyl ester The ester is obtained by chemical synthesis, and the related substances of 3-amino-2-butenoic acid methyl ester itself affect the quality of the raw material nitrendipine, which in turn affects the medication effect of the preparation nitrendipine tablet
No literature reports about impurities related to 3-amino-2-butenoic acid methyl ester have been found so far

Method used

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  • Detection method of impurities in 3-amino-2-butenoic acid methyl ester
  • Detection method of impurities in 3-amino-2-butenoic acid methyl ester
  • Detection method of impurities in 3-amino-2-butenoic acid methyl ester

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] Embodiment 1: the detection method of the purity of 3-amino-2-butenoic acid methyl ester

[0036] (1) Chromatographic conditions

[0037] Instrument: Agilent 7890B gas chromatograph;

[0038] Chromatographic column: modified polyethylene glycol filler (30m*0.53mm*0.5μm)

[0039] Injection volume: 1μl

[0040] Detector temperature: 230°C

[0041] Front inlet temperature: 230°C

[0042] Detector: FID

[0043] Split ratio: 30:1

[0044] Flow rate: 2ml / min

[0045] Heating program: The initial temperature is 90°C, keep for 5 minutes, then rise to 230°C at 10°C / min, and keep for 3 minutes.

[0046] (2) Sample preparation

[0047] Sample solution preparation: Weigh an appropriate amount of methyl β-aminocrotonate, dissolve and dilute with methanol to obtain a solution containing methyl β-aminocrotonate with a concentration of 100 mg / ml.

[0048] (3) Detection method

[0049] The autosampler extracts 1ul and injects it into the gas chromatograph, the chromatogram i...

Embodiment 2

[0063] Embodiment 2: the detection method of the purity of 3-amino-2-butenoic acid methyl ester

[0064] 1) Chromatographic conditions

[0065] Instrument: Agilent 7890B gas chromatograph;

[0066] Chromatographic column: modified polyethylene glycol filler (30m*0.53mm*0.5μm)

[0067] Injection volume: 1μl

[0068] Detector temperature: 230°C

[0069] Front inlet temperature: 120°C

[0070] Detector: FID

[0071] Split ratio: 30:1

[0072] Flow rate: 2ml / min

[0073] Heating program: the initial temperature is 80°C, keep it for 5 minutes, then raise it to 230°C at 10°C / min and keep it for 3 minutes.

[0074] (2) Sample preparation

[0075] Preparation of sample solution: Weigh an appropriate amount of methyl 3-amino-2-butenoate, dissolve and dilute with methanol to form a solution containing methyl 3-amino-2-butenoate at a concentration of 100 mg / ml.

[0076] (3) Detection method

[0077] The autosampler draws 1ul and injects it into the gas chromatograph.

[0078] ...

Embodiment 3

[0086] Embodiment 3: the detection method of the purity of 3-amino-2-butenoic acid methyl ester

[0087] 1) Chromatographic conditions

[0088] Instrument: Agilent 7890B gas chromatograph;

[0089] Chromatographic column: modified polyethylene glycol filler (30m*0.53mm*0.5μm)

[0090] Injection volume: 1μl

[0091] Detector temperature: 230°C

[0092] Front inlet temperature: 230°C

[0093] Detector: FID

[0094] Split ratio: 30:1

[0095] Flow rate: 2ml / min

[0096] Heating program: the initial temperature is 100°C, keep it for 5 minutes, then raise it to 230°C at 10°C / min and keep it for 3 minutes.

[0097] (2) Sample preparation

[0098] Preparation of sample solution: Weigh an appropriate amount of methyl 3-amino-2-butenoate, dissolve and dilute with methanol to form a solution containing methyl 3-amino-2-butenoate at a concentration of 100 mg / ml.

[0099] (3) Detection method

[0100] The autosampler draws 1ul and injects it into the gas chromatograph.

[010...

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Abstract

The invention provides a detection method of impurities in methyl 3-aminocrotonate. In the detection method, determination is carried out by using a gas chromatograph, and the method comprises the following specific detection steps: weighing a methyl 3-aminocrotonate sample, and preparing a methyl 3-aminocrotonate sample solution with concentration of 100mg / ml by using methanol; detecting impurities of the sample solution by using the gas chromatograph, wherein working conditions are that a chromatographic column filling agent is polyethyleneglycol; a sample feeding amount is 1 micro liter; atemperature of a front sample inlet is 120 to 230 DEG C; a temperature of a detector is 230 DEG C; the detector is an FID (Flame Ionization Detector); a split ratio is 30 to 1; a flow velocity is 2ml / min; a temperature rise program is carried out by adopting a gradient temperature rise manner, that is, initial temperature is 80 to 120 DEG C and is kept for 5 to 8 minutes, and then the temperatureis increased to 150 to 230 DEG C at a speed of 3 to 20 DEG C / min and is kept for 3 to 10 minutes. According to the detection method provided by the invention, impurity peak of the methyl 3-aminocrotonate can be effectively separated out, so that the purity detection sensitivity of the methyl 3-aminocrotonate is greatly improved, and the purity of the methyl 3-aminocrotonate can be simply, quicklyand stably detected.

Description

technical field [0001] The invention relates to the technical field of drug analysis, in particular to a detection method for impurities in 3-amino-2-butenoic acid methyl ester. Background technique [0002] The English name of 3-amino-2-butenoic acid methyl ester is Methyl 3-aminocrotonate, also known as β-aminocrotonate methyl ester, and its molecular formula is C 5 h 9 NO 2 , molecular weight is 115.13, chemical structure formula: 3-Amino-2-butenoic acid methyl ester is the starting material of the raw material drug nitrendipine, and the literature that can be consulted at present shows that the synthesis of the nitrendipine raw material drug uses 3-amino-2-butenoic acid methyl ester The ester is obtained by chemical synthesis, and the related substances of 3-amino-2-butenoic acid methyl ester itself affect the quality of the raw material nitrendipine, which in turn affects the medication effect of the preparation nitrendipine tablets. There is no literature report o...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/02G01N30/30
CPCG01N30/02G01N30/30G01N2030/3046
Inventor 吴桐刘钊金怡平袁金桥
Owner 湖南新领航检测技术有限公司