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2-ethyl-1,3-hexanediol purifying process and related substance detecting method

A detection method and purification method technology, applied in the field of medicine, can solve the problems of product quality impact, impact on the application of injection-grade excipients, etc., and achieve the effects of strict and accurate control, reducing the generation of impurities and ensuring quality

Active Publication Date: 2016-03-23
TIANJIN CHASE SUN PHARM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

It was recorded in USP18 of the "United States Pharmacopoeia", but it was not included in the subsequent "United States Pharmacopoeia", and this species was not included in the pharmacopoeias of other countries and the Chinese Pharmacopoeia
[0003] 2-Ethyl-1,3-hexanediol is very easy to introduce some impurities during the production process, which will affect the quality of the final product, especially its application as an injection grade excipient

Method used

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  • 2-ethyl-1,3-hexanediol purifying process and related substance detecting method
  • 2-ethyl-1,3-hexanediol purifying process and related substance detecting method
  • 2-ethyl-1,3-hexanediol purifying process and related substance detecting method

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Embodiment 1

[0099] Chromatographic conditions: DB624 chromatographic column with (6%) cyanopropylphenyl-(94%) methylpolysiloxane as the stationary liquid, the specification is 30m×0.53mm×3μm; the initial column temperature is 70°C, and it is maintained for 3 Minutes, the temperature was raised to 260°C at a rate of 20°C per minute, and maintained for 16 minutes; the split ratio was 10:1, the flow rate was 3ml / min, the inlet temperature was 250°C, and the detector temperature was 275°C.

[0100] Step 1, preparation of system suitability solution: the method is as follows: Weigh 2-ethyl-1,3-hexanediol and an appropriate amount of impurity 1, impurity 2, and impurity 3, and add absolute ethanol to prepare 2-ethyl-1 , The solution of 20mg / ml of 3-hexanediol and 0.1mg / ml of impurity 1, impurity 2, and impurity 3 is used as the system suitability solution;

[0101] Step 2, preparation of the test solution: the method is as follows: Weigh an appropriate amount of 2-ethyl-1,3-hexanediol, add abso...

Embodiment 2

[0107] Chromatographic conditions: DB624 chromatographic column with (6%) cyanopropylphenyl-(94%) methylpolysiloxane as the stationary liquid, the specification is 30m × 0.53mm × 3μm; the initial column temperature is 65 ° C, maintain 3 Minutes, the temperature was raised to 260°C at a rate of 20°C per minute, and maintained for 16 minutes; the split ratio was 10:1, the flow rate was 3ml / min, the inlet temperature was 250°C, and the detector temperature was 275°C.

[0108] Step 1, preparation of system suitability solution: the method is as follows: Weigh 2-ethyl-1,3-hexanediol and an appropriate amount of impurity 1, impurity 2, and impurity 3, and add absolute ethanol to prepare 2-ethyl-1 , The solution of 20mg / ml of 3-hexanediol and 0.1mg / ml of impurity 1, impurity 2, and impurity 3 is used as the system suitability solution;

[0109] Step 2, preparation of the test solution: the method is as follows: Weigh an appropriate amount of 2-ethyl-1,3-hexanediol, add absolute ethan...

Embodiment 3

[0115]Chromatographic conditions: DB624 chromatographic column with (6%) cyanopropylphenyl-(94%) methylpolysiloxane as the stationary liquid, the specification is 30m×0.53mm×3μm; the initial column temperature is 70°C, and it is maintained for 3 minutes, the temperature was raised to 260°C at a rate of 19°C per minute, and maintained for 16 minutes; the split ratio was 10:1, the flow rate was 3ml / min, the inlet temperature was 250°C, and the detector temperature was 275°C.

[0116] Step 1, preparation of system suitability solution: the method is as follows: Weigh 2-ethyl-1,3-hexanediol and an appropriate amount of impurity 1, impurity 2, and impurity 3, and add absolute ethanol to prepare 2-ethyl-1 , The solution of 20mg / ml of 3-hexanediol and 0.1mg / ml of impurity 1, impurity 2, and impurity 3 is used as the system suitability solution;

[0117] Step 2, preparation of the test solution: the method is as follows: Weigh an appropriate amount of 2-ethyl-1,3-hexanediol, add absol...

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Abstract

The invention belongs to the technical field of medicine, and particularly relates to a 2-ethyl-1,3-hexanediol purifying process and a related substance detecting method thereof. The purifying process is a calcium hydride reducing process. The detecting method comprises the following steps that 1, a system suitability solution is prepared, wherein an impurity1, an impurity 2, an impurity 3 and 2-ethyl-1,3-hexanediol are taken to be prepared into the system suitability solution; 2, a test solution is prepared, wherein 2-ethyl-1,3-hexanediol is taken to be prepared into the test solution; 3, a contrast solution is prepared, wherein the test solution is taken to be prepared into the contrast solution; , the system suitability solution, the contrast solution and the test solution are injected into a gaschromatograph, and a chromatogram is obtained; 5, according to the chromatogram of the system suitability solution, the contrast solution and the test solution, the content of know impurities, unknown impurities and total impurities in the test solution is obtained through calculation.

Description

technical field [0001] The invention belongs to the technical field of medicine, and in particular relates to a purification process of 2-ethyl-1,3-hexanediol and a detection method for related substances. Background technique [0002] 2-Ethyl-1,3-hexanediol is an almost colorless, slightly viscous oily liquid, used in boric acid complexing agents, pharmaceuticals, vehicles and solvents for paints, cosmetics, and insect repellents. It was included in the "United States Pharmacopoeia" USP18, but it was not included in the subsequent "United States Pharmacopoeia", and the pharmacopoeia of other countries and the Chinese Pharmacopoeia did not include this species. [0003] 2-Ethyl-1,3-hexanediol is very easy to introduce some impurities during the production process, which will affect the quality of the final product, especially its application as an injection grade excipient. [0004] According to the current research results, it is easy to introduce the following impurities ...

Claims

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Application Information

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IPC IPC(8): C07C31/20C07C29/88G01N30/02
CPCC07C29/88G01N30/02G01N2030/025C07C31/20
Inventor 刘黄刚孙福亮郭新荣董凯
Owner TIANJIN CHASE SUN PHARM CO LTD
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