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Method for detecting fluorobromomethane residues in bulk drugs

A kind of fluorobromomethane and detection method technology, applied in the field of analysis, can solve the problems of fluorobromomethane residue detection not being reported and included and the like

Pending Publication Date: 2020-10-09
TIANJIN PHARMA GROUP CORP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] After literature research, there is no report or record for the analysis method of fluorobromomethane and the detection of fluorobromomethane residues

Method used

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  • Method for detecting fluorobromomethane residues in bulk drugs
  • Method for detecting fluorobromomethane residues in bulk drugs
  • Method for detecting fluorobromomethane residues in bulk drugs

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0053] Embodiment 1 specificity test

Embodiment 11

[0055] Take methanol, acetone, acetonitrile, tetrahydrofuran, n-hexane, toluene, bromofluoromethane, dichloromethane, diethylamine, triethylamine, ethyl acetate, dimethylacetamide (DMA), and mesityl oxide respectively. Mix the API limit of each solvent by 100 times, add to N-methylpyrrolidone solvent and mix, as a specific mixed sample solution, take 2ml and put it in a 20ml headspace bottle, seal it for later use;

[0056] The above solutions were injected separately, and the chromatographic conditions were as follows:

[0057] Using gas chromatography, using DB-624 as a chromatographic column (6% cyanopropylphenyl-94% dimethyl polyoxysilane, 30m × 0.53mm × 3.0μm), the carrier gas is helium, and the carrier gas flow rate is 2.0 ml / min; use the headspace sampling method to inject samples, the headspace temperature is 30°C; the headspace time is 30min; the injection temperature is 200°C; the column temperature programming method is adopted, and the column temperature increase pro...

Embodiment 12

[0064] Take methanol, acetone, acetonitrile, tetrahydrofuran, n-hexane, toluene, bromofluoromethane, dichloromethane, diethylamine, triethylamine, ethyl acetate, dimethylacetamide (DMA), and mesityl oxide respectively. Mix the API limit of each solvent by 100 times, add to N-methylpyrrolidone solvent and mix, as a specific mixed sample solution, take 2ml and put it in a 20ml headspace bottle, seal it for later use;

[0065] The above solutions were injected separately, and the chromatographic conditions were as follows:

[0066] Using gas chromatography, using DB-624 as a chromatographic column (6% cyanopropylphenyl-94% dimethylpolyoxysilane, 30m × 0.53mm × 3.0μm), the carrier gas is helium, and the carrier gas flow rate is 2.2 ml / min; use the headspace sampling method to inject samples, the headspace temperature is 35°C; the headspace time is 28min; The column temperature was 35°C, maintained for 12.0 minutes, raised to 200°C at a rate of 8°C per minute, and maintained for 2...

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Abstract

The invention discloses a method for detecting fluorobromomethane residues in bulk drugs. The invention provides a method for detecting bromofluoromethane, and relates to a method for determining bromofluoromethane residues in API, which adopts gas chromatography, takes DB-624 as a chromatographic column and carrier gas as helium, adopts a headspace sample injection method for sample injection, adopts a column temperature programmed heating method, and selects a hydrogen flame ionization detector as a detector. The method has the beneficial effects that the headspace temperature is reduced to25-30 DEG C for detection, fluorobromomethane detected at the temperature can be completely vaporized, so that fluorobromomethane is prevented from reacting, volatilization of fluorobromomethane during direct sample introduction is avoided, and the detection precision is guaranteed.

Description

technical field [0001] The invention belongs to the field of analysis, in particular to a detection method for bromofluoromethane residues in raw materials. Background technique [0002] Bromofluoromethane (Bromofluoromethane, CAS: 373-52-4), also known as bromofluoromethane, is an important raw material for chemical production. It is mainly used to introduce fluoromethyl into chemical products. Other fluorohalomethylating reagents such as chlorofluoromethane. Bromofluoromethane is a colorless gas at room temperature with the molecular formula CH 2 BrF, molecular weight 112.93, density 1.76g / ml, very low boiling point, 17.8°C, easy to volatilize, should be kept frozen. Bromofluoromethane has a suspected genotoxic impurity structure, so precautions must be taken during use, and the residual amount of API should be strictly controlled. [0003] According to literature research, there are no reports or records on the analysis method of bromofluoromethane and the detection of...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/06G01N30/16G01N30/30G01N30/32G01N30/68G01N30/04
CPCG01N30/02G01N30/06G01N30/16G01N30/30G01N30/32G01N30/68G01N30/04G01N2030/324G01N2030/047
Inventor 刘晓茹强玉钗郭志强
Owner TIANJIN PHARMA GROUP CORP
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