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Method for analyzing alpha-fluoromethyl acrylate and related substances

A technology for methyl fluoroacrylate and related substances, which is applied in the field of analysis of methyl α-fluoroacrylate and related substances, can solve problems that need to be improved, and achieve good elution and separation effects, strong accuracy, and significant sensitivity Effect

Active Publication Date: 2016-04-27
湖北华世通生物医药科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] At present, the method for the analysis of methyl α-fluoroacrylate and its related substances still needs to be improved

Method used

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  • Method for analyzing alpha-fluoromethyl acrylate and related substances
  • Method for analyzing alpha-fluoromethyl acrylate and related substances
  • Method for analyzing alpha-fluoromethyl acrylate and related substances

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0050] Instrument: Agilent7890A gas chromatograph, FID detector

[0051] Chromatographic column: DB-wax (30m×0.32mm×0.25μm);

[0052] The temperature programming conditions are:

[0053] Heating rate (℃ / min)

[0054] Flow rate: 1.0mL / min

[0055] Detector temperature: 250°C

[0056] Inlet temperature: 240°C

[0057] Injection volume: 1μL

[0058] Split ratio: 50:1

[0059] Diluent: Acetonitrile

[0060] Derivatization reagent: add 60mg trifluoroacetic acid to 2g acetonitrile

[0061] Running time: 23.6min

[0062] Experimental steps:

[0063] BHT reference substance stock solution: about 80mg of BHT reference substance, accurately weighed, put in a 50mL volumetric flask, add diluent to dissolve and dilute to the mark, and shake well.

[0064] Sample and each component reference substance solution: Weigh about 80mg of α-methyl fluoroacrylate reference substance, weigh about 40mg each of MeOH, Toluene, MtBE, DMC, MFAc reference substance, weigh them accurately...

Embodiment 2

[0073] Instrument: Agilent7890A gas chromatograph, FID detector

[0074] Chromatographic column: DB-wax (30m×0.32mm×0.25μm);

[0075] The temperature programming conditions are:

[0076] Heating rate (℃ / min)

[0077] Flow rate: 1.0mL / min

[0078] Detector temperature: 250°C

[0079] Inlet temperature: 240°C

[0080] Injection volume: 1μL

[0081] Split ratio: 50:1

[0082] Diluent: Acetonitrile

[0083] Derivatization reagent: add 60mg trifluoroacetic acid to 2g acetonitrile

[0084] Runtime: 23.6 minutes

[0085] Experimental steps:

[0086] Impurity content reference substance solution: Take about 800mg of MFA reference substance, weigh it accurately, put it into a 10mL volumetric flask with 5mL diluent and 1mL derivatization reagent, add diluent to dissolve and dilute to the mark, shake well (80mg / mL ). Precisely pipette 1mL into a 200mL volumetric flask, add diluent to dilute to the mark, and shake well (0.4mg / mL).

[0087] Sample solution: Take about ...

Embodiment 3

[0095] Instrument: Agilent7890A gas chromatograph, FID detector

[0096] Chromatographic column: DB-wax (30m×0.32mm×0.25μm);

[0097] The temperature programming conditions are:

[0098] Heating rate (℃ / min)

temperature(℃)

Hold time (min)

running time (min)

40

8

8

5

60

0

12

25

230

5

23.8

[0099] Flow rate: 1.0mL / min

[0100] Detector temperature: 250°C

[0101] Inlet temperature: 230°C

[0102] Injection volume: 1μL

[0103] Split ratio: 50:1

[0104] Thinner: Acetone

[0105] Derivatization reagent: add 100mg trifluoroacetic acid to 2g acetone

[0106] Running time: 23.8min

[0107] Experimental procedure: Accurately weigh about 200 mg of the MFA reaction solution, add 1 mL of derivatization reagent and 1 mL of diluent, shake well, and filter to obtain the product.

[0108] Conclusion: under this chromatographic condition, the gas chromatogram of gained α-fluoromethyl acrylate react...

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Abstract

The invention discloses a method for analyzing alpha-fluoromethyl acrylate and related substances. Chromatographic conditions are as follows: a polar capillary chromatographic column is employed as a chromatographic column; a temperature control mode is programmed heating, a split mode is employed for sample introduction and nitrogen is used as carrying gas; a flame ionization detector is used as a detector; and alpha-fluoromethyl acrylate and a reference substance are prepared from a first solvent and a second solvent, wherein the first solvent is acetone and / or acetonitrile and the second solvent is a derivatization reagent. Solutions of alpha-fluoromethyl acrylate and the reference substance are placed in a sample injector; and after balancing, a sample or reference substance is injected into a gas chromatograph so as to accomplish determination of alpha-fluoromethyl acrylate and the related substances. With the method, alpha-fluoromethyl acrylate and impurities produced during synthesis of alpha-fluoromethyl acrylate can be rapidly and highly-efficiently separated under same chromatographic conditions, so synthesis reaction process and product quality are effectively controlled. The detection method is convenient to operate, has high sensitivity and good accuracy and can comprehensively and effectively control product quality.

Description

technical field [0001] The invention belongs to the technical field of drug analysis, in particular, the invention relates to a method for analyzing methyl alpha-fluoroacrylate and its related substances. Background technique [0002] In recent years, α-methyl fluoroacrylate and its analogues have been used more and more in the pharmaceutical and material industries, and the demand has also increased accordingly. In particular, polymers made from acrylates are widely used in the information industry; in the field of medicine, polymers prepared from α-fluoromethyl acrylate can be prepared after being combined with some highly active drugs. As a new drug, it enters the human body as a delivery medium, and excretes some excess potassium and sodium ions from the human body. [0003] [0004] Wherein, R and X are each independently selected from any one of the following groups: C 1 -C 3 Alkyl, X is a halogen group. [0005] As one of the compounds shown in formula I, α-met...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/88
CPCG01N30/88
Inventor 林娟戚争春钱丽娜王念
Owner 湖北华世通生物医药科技有限公司
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