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Analysis and separation method of related substance L-2-aminobutyric acid in D-2-aminobutanol

A separation method and aminobutanol technology, applied in the field of drug analysis, can solve problems such as difficulty, difficulty in realization, and easy generation of by-products, and achieve the effect of good separation effect and good specificity

Pending Publication Date: 2021-06-15
WUHAN WUYAO PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] There is a small amount of related substance L-2-aminobutyric acid in D-2-aminobutanol, although the chiral high-performance liquid chromatography (chiral-HPLC) method can accurately detect the stereoisomer content of chiral compounds, but due to The molecular structure of 2-aminobutanol contains a primary amine and a hydroxyl group. There are no conjugated groups and no UV-absorbing functional groups in the molecular structure, which makes it very difficult to establish a convenient, fast and reliable optical purity analysis method.
Patent ZL201610043273.3 and patent application 201610043277.1 both use derivatization reagents and 2-aminobutanol for derivatization reaction to generate derivatives with ultraviolet absorption, and then use high-performance liquid chromatography for detection. However, the derivatization method has complicated steps , Derivatives are prone to produce by-products and other defects
If the GC method is used to detect D-2-aminobutanol, the impurity aminobutyric acid is solid, and it is difficult to realize gasification

Method used

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  • Analysis and separation method of related substance L-2-aminobutyric acid in D-2-aminobutanol
  • Analysis and separation method of related substance L-2-aminobutyric acid in D-2-aminobutanol
  • Analysis and separation method of related substance L-2-aminobutyric acid in D-2-aminobutanol

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0056] Stationary phase: silica gel G (0.25mm);

[0057] Developing agent: anhydrous methanol, acetonitrile and ammonia water, the volume ratio is 6.7:2.6:0.7;

[0058] Expanded height: reach 3 / 4 of the height of the thin-layer board;

[0059] Chromogenic agent: ninhydrin test solution;

[0060] The preparation method is: take 1.0g of ninhydrin, add 50ml of ethanol to dissolve, then add 10ml of glacial acetic acid, and shake well.

[0061] Operation process:

[0062] (1) Prepare the test solution; take 0.5g of the test product to a 10ml volumetric flask, dissolve in a small amount of purified water, dilute with methanol and be constant to the mark, and prepare a solution with a concentration of 50mg / ml;

[0063] (2) Resolution solution: Take 5 mg of L-2-aminobutyric acid reference substance and 50 mg of D-2-aminobutanol reference substance into the same 10ml volumetric flask, dissolve in a small amount of purified water, dilute with methanol to volume, and prepare A resolu...

Embodiment 2

[0067] Stationary phase: silica gel G (0.25mm);

[0068] Developing agent: anhydrous methanol, acetonitrile and ammonia water, the volume ratio is 4.5:4.5:1;

[0069] Expanded height: reach 3 / 4 of the height of the thin-layer board;

[0070] Chromogen: ninhydrin test solution (preparation method is the same as in Example 1).

[0071] Operation process:

[0072] (1) Prepare the test solution; take 0.5g of the test product to a 10ml volumetric flask, dissolve in a small amount of purified water, dilute with methanol and be constant to the mark, and prepare a solution with a concentration of 50mg / ml;

[0073] (2) Resolution solution: Take 5 mg of L-2-aminobutyric acid reference substance and 50 mg of D-2-aminobutanol reference substance into the same 10ml volumetric flask, dissolve in a small amount of purified water, dilute with methanol to volume, and prepare A resolution solution containing 5 mg / ml of D-2-aminobutanol and 0.5 mg / ml of L-2-aminobutyric acid;

[0074] (3) Sp...

Embodiment 3

[0077] Stationary phase: silica gel G (0.25mm);

[0078] Developing agent: anhydrous methanol, acetonitrile and ammonia water, the volume ratio is 2:7:1;

[0079] Expanded height: reach 3 / 4 of the height of the thin-layer board;

[0080] Chromogen: ninhydrin test solution (preparation method is the same as Example 1).

[0081] Operation process:

[0082] (1) Prepare the test solution; take 0.5g of the test product to a 10ml volumetric flask, dissolve in a small amount of purified water, dilute with methanol and be constant to the mark, and prepare a solution with a concentration of 50mg / ml;

[0083] (2) Resolution solution: Take 5 mg of L-2-aminobutyric acid reference substance and 50 mg of D-2-aminobutanol reference substance into the same 10ml volumetric flask, dissolve in a small amount of purified water, dilute with methanol to volume, and prepare A resolution solution containing 5 mg / ml of D-2-aminobutanol and 0.5 mg / ml of L-2-aminobutyric acid;

[0084] (3) Spot 1 μl...

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Abstract

The invention belongs to the field of pharmaceutical analysis and relates to an analysis and separation method of a related substance L-2-aminobutyric acid in D-2-aminobutanol. According to the method, a thin-layer chromatography is adopted for analysis or separation, a stationary phase of the thin-layer chromatography is silica gel G, and a developing solvent is a mixed solvent containing absolute methanol, acetonitrile and ammonia water. The method disclosed by the invention is simple and rapid, can be carried out without expensive experimental equipment, has a good separation effect and avoids a tailing condition, can detect and effectively separate L-2-aminobutyric acid, and has good specificity; and the lowest detection concentration of the method can reach 0.1%.

Description

technical field [0001] The invention relates to the field of drug analysis, in particular to a method for analyzing and separating L-2-aminobutyric acid, a related substance in D-2-aminobutanol. Background technique [0002] 2-aminobutanol (2-amino-n-butanol, 2-Amino-1-butanol), also known as 2-amino-1-butanol, butanol-2-amine, is a colorless liquid. 2-amino-n-butanol has chirality and belongs to chiral compounds, specifically including D or L configuration, and 2-amino-n-butanol with D or L configuration is widely used as chemical raw material intermediates, such as in ethyl hydrochloride In the synthesis of butanol, it is an important starting material. [0003] There is a small amount of related substance L-2-aminobutyric acid in D-2-aminobutanol, although the chiral high-performance liquid chromatography (chiral-HPLC) method can accurately detect the stereoisomer content of chiral compounds, but due to The molecular structure of 2-aminobutanol contains a primary amine ...

Claims

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Application Information

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IPC IPC(8): G01N30/90G01N30/74G01N30/06
CPCG01N30/90G01N30/74G01N30/06
Inventor 赵涛涛徐煜涵王成张伟肖应国张琦
Owner WUHAN WUYAO PHARMA
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