Method for analyzing and determining methyl trifluoropyruvate

A technology of methyl trifluoropyruvate and methyl pyruvate, applied in the field of analysis and determination of methyl trifluoropyruvate, can solve the problems of expensive instruments, unsuitable for routine analysis of enterprises, difficult quantitative analysis, etc., and the method is simple , Test the effect of low price and high practical value

Inactive Publication Date: 2016-06-08
TIANJIN CHANGLU CHEM NEW MATERIAL CO LTD
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] In order to solve the above technical problems, the present invention provides a method for the analysis and determination of methyl trifluoropyruvate, so as to solve the problems existing in the existing technology that it is difficult

Method used

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  • Method for analyzing and determining methyl trifluoropyruvate
  • Method for analyzing and determining methyl trifluoropyruvate
  • Method for analyzing and determining methyl trifluoropyruvate

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Embodiment

[0023] as attached figure 1 And attached figure 2 shown

[0024] The invention provides a method for the analysis and determination of methyl trifluoropyruvate. The methyl trifluoropyruvate is analyzed by gas chromatography, and the content of methyl trifluoropyruvate is directly quantitatively determined by the area normalization method, which specifically includes the following steps:

[0025] S101: Take a sample of methyl trifluoropyruvate;

[0026] S102: use a chromatograph for chromatographic analysis;

[0027] S103: Using a formula to calculate the content of methyl trifluoropyruvate.

[0028] Further, in S101, 0.2 uL of methyl trifluoropyruvate sample is specifically taken.

[0029] Further, in S102, the 0.2 uL sample of methyl trifluoropyruvate that was taken out was subjected to chromatographic analysis with a chromatographic instrument, and the chromatographic analysis temperature rise program specifically adopted an initial temperature of 40°C, kept for 1min, a...

specific Embodiment

[0037] instrument

[0038] Agilent 7820 chromatograph produced in the United States

[0039] Chromatographic conditions

[0040] Detector: FID (Flame Ionization Detector)

[0041] Column: HP-5

[0042] Split ratio: 100:1

[0043] Gas velocity: 2mL / min

[0044] Column temperature rise program: 40°C / 1min→10°C / min→260°C / 1min

[0045] Injector: 250°C

[0046] Detector: 250°C

[0047] sample analysis

[0048] Sampling 0.2uL was carried out chromatographic analysis, and the content of methyl trifluoropyruvate was obtained according to the following formula.

[0049] Methyl trifluoropyruvate (%)=A / ∑A(1)

[0050] In the formula: A is the peak area of ​​methyl trifluoropyruvate

[0051] ΣA is the total area of ​​each peak.

[0052] Such as figure 1 Among them, the peak area of ​​methyl trifluoropyruvate is 56780240, the peak area of ​​hydrate is 379565, and the peak area of ​​methyl trifluoroacetate is 821365, so the content of methyl trifluoropyruvate is:

[0053] Peak ar...

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Abstract

The invention provides a method for analyzing and determining methyl trifluoropyruvate. Problems that quantitative analysis is hard to carry out through a chromatographic detection method and infrared analysis, and a nuclear magnetic resonance instrument is expensive and is not suitable for routine analysis for an enterprise in the prior art is solved. In the method, methyl trifluoropyruvate is determined through gas chromatography, and the content of methyl trifluoropyruvate is subjected to direct quantitative determination through area normalization. The method comprises: taking a methyl trifluoropyruvate sample; using a chromatographic instrument for chromatographic analysis; and using a formula to calculate the content of methyl trifluoropyruvate. The method has the beneficial effects that a gas chromatographic analytical method for direct quantitative determination is established to obtain a stable analysis result, and research and production of methyl trifluoropyruvate can be directed through the method. The method is simple and reliable, and is low in determination price. The method is suitable for routine analysis for an enterprise and has high practical value.

Description

technical field [0001] The invention belongs to the field of chemical analysis, and in particular relates to an analysis and determination method of methyl trifluoropyruvate. Background technique [0002] Methyl trifluoropyruvate is an important trifluoromethylation reagent that can be used in the synthesis of a variety of novel fluorine-containing drugs, including anti-inflammatory, anticancer and antiviral drugs. In the production process, due to the existence of traces of water, hydrates that are very close to the boiling point of methyl trifluoropyruvate will be formed during the production process, and there are a small amount of other impurities such as methyl trifluoroacetate. Due to the existence of these impurities, it will Reduces the effectiveness of trifluoromethylating reagents. Therefore, high-purity methyl trifluoropyruvate is required in production. However, it is difficult to quantitatively analyze it using chromatographic detection methods and infrared an...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/68
CPCG01N30/02G01N30/68G01N2030/025
Inventor 闫锐郭海强相继欣肖山
Owner TIANJIN CHANGLU CHEM NEW MATERIAL CO LTD
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