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HPLC analytical method for chirality purity of 2-amino butanol

An aminobutanol, chiral purity technology, applied in analytical materials, material separation, measurement devices, etc., can solve the problems of difficult optical purity analysis methods, and achieve the effects of convenient standardized operation, high sensitivity and good reproducibility

Inactive Publication Date: 2016-04-20
HEBEI UNIVERSITY OF SCIENCE AND TECHNOLOGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The molecular structure of 2-aminobutanol contains a primary amine and a hydroxyl group, and there is no UV-absorbing functional group, which makes it very difficult to establish a convenient, fast and reliable optical purity analysis method

Method used

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  • HPLC analytical method for chirality purity of 2-amino butanol
  • HPLC analytical method for chirality purity of 2-amino butanol
  • HPLC analytical method for chirality purity of 2-amino butanol

Examples

Experimental program
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Effect test

Embodiment 1

[0032] Example 1: Liquid chromatography analysis of derivatives of (R)-α-methyl-2-naphthaleneacetyl chloride and (RS)-2-aminobutanol

[0033] Take (RS)-2-aminobutanol 3.09g (0.03mol), dissolve it in 50mL of dichloromethane, stir at 30°C, slowly add (R)-α-methyl-2-naphthaleneacetyl chloride 19.67g (0.09 mol). The reaction was monitored by TLC, and evaporated to dryness after the reaction to obtain (R)-α-methyl-2-naphthaleneacetyl chloride and (RS)-2-aminobutanol derivatives.

[0034] (R)-α-methyl-2-naphthalene acetyl chloride and (RS)-2-aminobutanol derivatives were dissolved in mobile phase and then detected and analyzed by high performance liquid chromatography. Liquid chromatography conditions: Dima C18 chromatographic column, the mobile phase is 80% methanol-20% hydrochloric acid solution, the molar concentration of the hydrochloric acid solution is 0.2mol / L, and the pH value is 4.5. The UV detection wavelength is 254nm, the flow rate is 1.0mL / min, the column temperature ...

Embodiment 2

[0037] Embodiment 2: The derivatization condition investigation test of 2-aminobutanol and (R)-α-methyl-2-naphthaleneacetyl chloride

[0038] 2-1: Take 3.09g (0.03mol) of (RS)-2-aminobutanol, dissolve it in 30mL of 1,2-dichloroethane, stir at 60°C, and slowly add (R)-α-methyl-2 - Naphthaleneacetyl chloride 218.6 g (0.1 mol). The reaction was monitored by TLC, and evaporated to dryness after the reaction to obtain (R)-α-methyl-2-naphthaleneacetyl chloride and (RS)-2-aminobutanol derivatives.

[0039] (R)-α-methyl-2-naphthalene acetyl chloride and (RS)-2-aminobutanol derivatives were dissolved in mobile phase and then detected and analyzed by high performance liquid chromatography. Liquid chromatography conditions: Dima C18 chromatographic column, the mobile phase is 80% methanol-20% hydrochloric acid solution, the molar concentration of the hydrochloric acid solution is 0.2mol / L, and the pH value is 4.5. The ultraviolet detection wavelength is 254nm, the flow rate is 1.0mL / mi...

Embodiment 3

[0051] Embodiment 3: chromatographic condition investigation test

[0052] (1) Derivatization

[0053] Take (RS)-2-aminobutanol 3.09g (0.03mol), dissolve it in 50mL of dichloromethane, stir at 30°C, slowly add (R)-α-methyl-2-naphthaleneacetyl chloride 19.67g (0.09 mol). The reaction was monitored by TLC, and evaporated to dryness after the reaction to obtain (R)-α-methyl-2-naphthaleneacetyl chloride and (RS)-2-aminobutanol derivatives.

[0054] (2) Separate and detect (R)-α-methyl-2-naphthaleneacetyl chloride and (RS)-2-aminobutanol derivatives using the following different chromatographic conditions

[0055] A. (R)-α-methyl-2-naphthalene acetyl chloride and (RS)-2-aminobutanol derivatives were dissolved in mobile phase and then detected and analyzed by high performance liquid chromatography. Liquid chromatography conditions: Dima C18 chromatographic column, the mobile phase is 40% acetonitrile-60% hydrochloric acid solution, the concentration of the hydrochloric acid solu...

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Abstract

The invention belongs to the technical field of pharmaceutical analysis and specifically relates to a HPLC (High Performance Liquid Chromatography) analytical method for chirality purity of 2-amino butanol. The method comprises the following steps: by taking R-alpha-methyl-2-naphthalene acetylchloride as a derivatization reagent, performing quick double-derivatization reaction with 2-amino butanol, generating ultraviolet absorption ramifications, and then determining the nature, quantity and chirality purity of 2-amino butanol by using HPLC and ultraviolet. According to the method, the derivatization reaction is quick and mild in reaction conditions; the detection sensitivity is high; the repeatability is excellent; the method can be used for effectively detecting the chirality purity of 2-amino butanol; the standardizing operation is easily performed; the method has practical application value and practical significance.

Description

technical field [0001] The invention belongs to the technical field of drug analysis, in particular to an HPLC analysis method for the chiral purity of 2-aminobutanol. Background technique [0002] (R)-2-aminobutanol is an important intermediate for the synthesis of dexlansoprazole. U.S. FDA approved on January 30, 2009 the listing of the esophagitis treatment new drug dexlansoprazole (common name Dexlansoprazole) developed by Japan's Takeda Pharmaceutical Company. The drug is an enantiomer of the proton pump inhibitor lansoprazole, also known as dexlansoprazole, and is used to treat heartburn and varying degrees of erosive esophagus associated with non-erosive gastroesophageal reflux disease Inflammation, clinically indicated that the drug has low toxicity and side effects and is well tolerated by patients. [0003] Dexlansoprazole has a chiral center which is introduced by (R)-2-aminobutanol, if the optical purity of (R)-2-aminobutanol is lower, there will be another is...

Claims

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Application Information

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IPC IPC(8): G01N30/89
CPCG01N30/89
Inventor 孙凤霞周蒙孔飞飞张琛王美玲蒲寒莹
Owner HEBEI UNIVERSITY OF SCIENCE AND TECHNOLOGY
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