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Purity analysis method and chiral analysis method of 1-decyne-5 alcohol

An analytical method, decyne technology, applied in the field of analysis and detection, can solve the problems that the purity detection method and chirality detection method of 1-decyne-5-ol alkynyl alcohol compounds are not given, and achieve good peak shape and separation good effect

Pending Publication Date: 2021-12-31
SHANGHAI LINKCHEM TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0007] However, the purity detection method and chirality detection method of alkynyl alcohol compounds such as 1-decyne-5 alcohol are not given in this patent document and other prior art

Method used

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  • Purity analysis method and chiral analysis method of 1-decyne-5 alcohol
  • Purity analysis method and chiral analysis method of 1-decyne-5 alcohol
  • Purity analysis method and chiral analysis method of 1-decyne-5 alcohol

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Embodiment 1

[0034] This embodiment provides a method for analyzing the purity of 1-decyne-5 alcohol. The analysis method is a gas chromatography method. The conditions are shown in Table 1:

[0035] Table 1 Example 1 Gas Chromatography Condition Table

[0036]

[0037] Such as figure 1 As shown, the method provided in this example can effectively separate and detect 1-decyn-5 alcohol, and confirm its content.

Embodiment 2

[0039] This embodiment provides a chiral analysis method for 1-decyne-5 alcohol, which is a gas chromatography method, and the sample detected in this embodiment is a 0.5% spiked sample, and the gas chromatography conditions are as follows: Table 2 shows:

[0040] Table 2 Example 2 gas chromatography condition table

[0041]

[0042]

[0043] Such as figure 2 As shown, (S)-1-decyn-5 alcohol and (R)-1-decyn-5 alcohol can be effectively separated by using the gas chromatography provided in this example, the peak shape is good, and the resolution can reach 1.71. The standard recovery rate was 112.2%.

Embodiment 3

[0045] This embodiment provides a chiral analysis method of 1-decyne-5 alcohol, which is a gas chromatography method, and the sample detected in this embodiment is a 0.5% standard-added sample, and the gas chromatography conditions are the same as The gas chromatography conditions in Example 2 are basically the same, the only difference is that the initial temperature of the column temperature is 60°C.

[0046] Such as image 3 As shown, the gas chromatography method provided by this embodiment can effectively separate (S)-1-decyne-5 alcohol and (R)-1-decyne-5 alcohol, the degree of separation can reach 1.90, and the recovery of standard addition is 92.4%, but compared with the method provided in Example 2, the detection time is too long.

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Abstract

The invention provides a purity analysis method and a chiral analysis method of 1-decyne-5 alcohol, and belongs to the field of analysis and detection. According to the purity analysis method of the 1-decyne-5 alcohol, provided by the invention, the purity of the 1-decyne-5 alcohol can be accurately and efficiently detected by adopting the gas chromatographic method and proper gas chromatographic conditions. According to the chiral analysis method for the 1-decyne-5 alcohol provided by the invention, the gas chromatography is adopted, the initial temperature of the column temperature is controlled between 60 DEG C and 80 DEG C, and the flow rate of the carrier gas column is controlled between 2mL / min and 4mL / min, so that two chiral isomers of the 1-decyne-5 alcohol can be effectively separated in a spectrogram, and the method is good in peak pattern and separation degree.

Description

technical field [0001] The invention relates to the field of analysis and detection, in particular to a purity analysis method and a chiral analysis method of 1-decyne-5 alcohol. Background technique [0002] Treprostinil is a prostaglandin drug developed by United Pharmaceuticals for the treatment of pulmonary arterial hypertension. Treprostinil injection is one of the most effective injection preparations for the treatment of pulmonary arterial hypertension in the prior art. The drug has good stability and long half-life. It is mainly administered by subcutaneous continuous infusion, and can also be administered by intravenous injection. The clinical trial data show that the drug has definite clinical curative effect, and its safety is superior to other marketed prostacyclin analogues. [0003] According to the Chinese patent report whose patent publication number is CN104892555 A, the intermediate of treprostinil can be synthesized through the following reaction pathway:...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/06G01N30/68
CPCG01N30/02G01N30/06G01N30/68
Inventor 陆茜付杨杰陈晶晶
Owner SHANGHAI LINKCHEM TECH CO LTD
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