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Indirect test method for Miglitol purity

A technology of miglitol and purity, which is applied in the field of indirect testing methods for the purity of miglitol, which can solve the problems of large molecular weight, complicated operation, high equipment requirements, etc., and achieve the effect of simple test method, accurate test result and low cost

Inactive Publication Date: 2011-11-23
ZHEJIANG UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] Since miglitol is a polyhydroxy compound, the intermolecular force is strong (mainly hydrogen bonds), and the molecular weight is large, the volatility is low, and the polarity is strong, so it cannot be directly detected by gas chromatography (GC).
At present, high-performance liquid chromatography (HPLC) is mostly used in the detection of miglitol, which has the following shortcomings: (1) Miglitol is picky about the detector, because it has no ultraviolet absorption, so it cannot be used with sensitive ultraviolet light. (2) Parallax refractive index detectors are generally used now, but they have the disadvantages of low sensitivity, being easily affected by ambient temperature and mobile phase, resulting in large errors in detection results; (3) This method requires high equipment and is complicated to operate

Method used

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  • Indirect test method for Miglitol purity
  • Indirect test method for Miglitol purity
  • Indirect test method for Miglitol purity

Examples

Experimental program
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Effect test

Embodiment 1

[0026] Embodiment 1, a kind of indirect test method of Miglitol purity, comprises the following steps:

[0027] 1) Add 1.86g of Miglitol white powder to be tested (pure product), 17ml of acetic anhydride, 1ml of anhydrous pyridine into a 50ml three-necked flask, stir mechanically, reflow the air condenser, control the heating temperature to 93-97°C, and react After 2 hours, the reaction was stopped to obtain an esterification reaction solution containing acetic acid-β-(3,4,5-triacetoxy-2-acetoxymethyl-1-piperidine)-ethyl ester (about 20-25ml) .

[0028] 2), the above-mentioned esterification reaction solution is directly sampled and detected, and the gas chromatograph used is equipped with a hydrogen flame monitor and a temperature program to obtain Base-1-piperidine)-ethyl ester, light components (acetic acid generated, unreacted acetic anhydride, unreacted catalyst anhydrous pyridine), the peak area is normalized after removing the light components After chemical treatment...

Embodiment 2

[0037] Embodiment 2, a kind of indirect test method of Miglitol purity, comprises the following steps:

[0038] 1) Add 1.86g of Miglitol white powder to be tested (composed of 1.60g of pure Miglitol + 0.26g of sorbitol) into a 50ml three-necked bottle, 20ml of acetic anhydride, stir mechanically, and reflux the air condenser to control Heating temperature is 93~97°C, react for 2 hours, stop the reaction, and obtain acetic acid-β-(3,4,5-triacetoxy-2-acetoxymethyl-1-piperidine)-ethyl ester (structural formula is as follows: 1) The esterification reaction solution.

[0039]2), the above-mentioned esterification reaction solution is directly sampled and detected, and the gas chromatograph used is equipped with a hydrogen flame monitor and a temperature program to obtain Base-1-piperidine)-ethyl ester, and impurity (sorbitol ester), light components (including acetic acid generated, unreacted acetic anhydride) gas chromatogram. After removing the light component, the peak area is...

Embodiment 3

[0041] Embodiment 3, an indirect test method of the purity of Miglitol, the 1.86g white powder of Miglitol to be tested in Example 2 is changed to be composed of 1.50g pure Miglitol+0.36g sorbitol , all the other contents are with embodiment 2; Gained result is as follows:

[0042] Acetate-β-(3,4,5-triacetoxy-2-acetoxymethyl-1-piperidine)-ethyl ester mass percentage content is 78.6%, because miglitol is all converted into acetic acid- β-(3,4,5-triacetoxy-2-acetoxymethyl-1-piperidine)-ethyl ester, the calculated purity of miglitol was 81.2%.

[0043] The actual purity of the miglitol sample to be tested was 80.6%, and the test accuracy was 99.3%.

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Abstract

The invention discloses an indirect testing method of the purity quotient of miglitol, comprising the following steps: 1) the miglitol to be tested is taken as substrate, and acetic anhydride is taken as acetylation reagent to have acetylation reaction, so that esterification reaction liquid containing acetic acid-beta-(3, 4, 5-triacetyl oxygroup-2-acetoxyl methyl-1-piperidine)-ethyl ester is obtained; or the miglitol to be tested is taken as substrate, propionic andydride is taken as acetylation reagent, and acetylation reaction is carried out under the catalysis of anhydrous pyridine, so that the esterification reaction liquid containing the acetic acid-beta-(3, 4, 5-triacetyl oxygroup-2-acetoxyl methyl-1-piperidine)-ethyl ester is obtained; 2) gas chromatography is carried out on the esterification reaction liquid, and the retaining time and the peak area of all the components in gas chromatograph can be obtained; after the peak area of the light components is eliminated, the purity quotient of the obtained miglitol is calculated according to normalization method. The indirect testing method has the characteristics of simple testing method and accurate testing result.

Description

technical field [0001] The invention relates to an indirect test method for the purity of miglitol. Background technique [0002] Miglitol is a type II diabetes inhibitory drug, its structure is (I): [0003] [0004] Since miglitol is a polyhydroxy compound with strong intermolecular forces (mainly hydrogen bonds), large molecular weight, low volatility, and strong polarity, it cannot be directly detected by gas chromatography (GC). At present, high-performance liquid chromatography (HPLC) is mostly used in the detection of miglitol, which has the following shortcomings: (1) Miglitol is picky about the detector, because it has no ultraviolet absorption, so it cannot be used with sensitive ultraviolet light. (2) Parallax refractive index detectors are generally used now, but they have the disadvantages of low sensitivity and being easily affected by ambient temperature and mobile phase, resulting in large errors in detection results; (3) This method has high requirements...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/02C07D211/46
Inventor 陈新志张旭王帅
Owner ZHEJIANG UNIV
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