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Preparation method of acarbose impurity reference substance

A technology of impurity reference substance, acarbose, which is applied in the preparation of test samples, sampling, and measuring devices, etc., and can solve the problems of not being able to provide acarbose quality control impurity reference substance preparation methods, etc.

Pending Publication Date: 2021-11-19
HANGZHOU ZHONGMEI HUADONGPHARMACEUTICAL JIANGDONG CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Existing methods and literature do not carry out detailed impurity preparation, and cannot provide the impurity reference substance preparation method that must be used in acarbose quality control and impurity research

Method used

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  • Preparation method of acarbose impurity reference substance
  • Preparation method of acarbose impurity reference substance
  • Preparation method of acarbose impurity reference substance

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0041] 1. Acarbose Impurity I Extraction

[0042] (1) The acarbose impurity I was enriched from the acarbose sample with a LC silica gel pre-column with a particle size of 20-45 μm. Take 300mL of acarbose impurity I enrichment solution, adjust the pH to 3.0-6.0 with dilute hydrochloric acid, concentrate to 30mg / mL by distillation under reduced pressure, then adjust the pH to 7.0-10.0 with diluted ammonia water, and finally filter with a 0.45μm filter membrane Obtain I miscellaneous concentrate.

[0043] (2) Twice in a row with C 18 Packing separation and purification conditions are used to elute the impurity concentrate. C 18 Packing separation and purification conditions are: instrument: DAC50 preparative liquid chromatography system (Beijing Innovation Tongheng Technology Co., Ltd.); chromatographic column: WelchXtimate C 18 , 10μm filler packing 300g; mobile phase: methanol-water (containing 0.1% NH 3 ) solution=8-92 (V / V); flow rate: 50mL / min; injection volume: 10mL; ...

Embodiment 2

[0060] 1. Acarbose Impurity II Extraction

[0061] (1) The acarbose impurity II was enriched from the acarbose sample with a LC silica gel pre-column with a particle size of 20-45 μm. Take 300mL of acarbose impurity II enrichment solution, adjust the pH to 3.0-6.0 with dilute hydrochloric acid, distill and concentrate under reduced pressure to 30mg / mL, then adjust the pH to 7.0-10.0 with diluted ammonia water, and finally filter with a 0.45μm filter membrane Get a concentrate.

[0062] (2) Twice in a row with C 18 Packing separation and purification conditions The impurity II concentrate is eluted, and the fraction containing acarbose impurity II is collected. C 18 Packing separation and purification conditions: instrument: DAC50 preparative liquid chromatography system (Jiangsu Hanbang Technology Co., Ltd.); chromatographic column: Welch Xtimate C 18 , 10μm filler packing 300g; mobile phase: methanol-water (containing 0.1% NH 3 ) solution=8-92 (V / V); flow rate: 50mL / min;...

Embodiment 3

[0079] 1. Extraction of acarbose impurity Ⅲ

[0080] (1) The acarbose impurity III was enriched from the acarbose sample with a LC silica gel pre-column with a particle size of 20-45 μm. Take 300mL of acarbose impurity III enrichment solution, adjust the pH to 3.0-6.0 with dilute hydrochloric acid, concentrate to 30mg / mL by distillation under reduced pressure, then adjust the pH to 7.0-10.0 with diluted ammonia water, and finally filter with a 0.45μm filter membrane Get a concentrate.

[0081] (2) with C 18 The packing separation and purification conditions elute the concentrated solution, and collect the fraction containing acarbose impurity III. C 18 Packing separation and purification conditions: instrument: DAC50 preparative liquid chromatography system (Jiangsu Hanbang Technology Co., Ltd.); chromatographic column: Welch Xtimate C 18 , 10μm filler packing 300g; mobile phase: methanol-water (containing 0.1% NH 3 ) solution=8-92 (V / V); flow rate: 50mL / min; injection vo...

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Abstract

The invention discloses a preparation method of an acarbose impurity reference substance and belongs to the technical field of pharmaceutical analysis. According to the method, separation and purification, freeze drying, content detection, structure confirmation and standardization are carried out on the four acarbose impurities I, II, III and IV by adopting multiple technologies such as preparative liquid chromatography, ultraviolet absorption spectrum, infrared absorption spectrum, time-of-flight mass spectrum (TOF-MS), nuclear magnetic resonance spectrum (NMR), freeze dryer, quantitative nuclear magnetic detection and the like. The four impurities can be used as impurity reference substances in quality detection of acarbose raw material medicines and preparations. The invention provides a separation and purification method of acarbose impurities, which is a universal separation method of an acarbose impurity reference substance, can be used for purification and preparation of other related substances of acarbose, and solves a problem of lack of impurity reference substances in current acarbose quality control and impurity research.

Description

technical field [0001] The invention belongs to the field of drug analysis, and in particular relates to a preparation method of an acarbose impurity reference substance. Background technique [0002] Acarbose is O-4,6-dideoxy-4-[1S,4R,5S,6S]-4,5,6-trihydroxy-3-(hydroxymethyl)-2-cyclohexyl En-1-amino]-α-D-glucopyranosyl-(1→4)-O-α-D-glucopyranosyl-(1→4)-α-D-glucopyranosyl, As an α-glucosidase inhibitor, it competitively inhibits glucoside hydrolase (maltase, isomaltase, glucoamylase and sucrase) in the intestinal tract, reduces the decomposition of polysaccharides and sucrose into glucose, and makes the absorption of sugar corresponding Slow down, has the effect of lowering blood sugar after meals, thereby alleviating postprandial hyperglycemia and achieving the effect of lowering blood sugar. [0003] Acarbose is a raw material for oral preparations, and the impurities contained in it will affect the safety of the product, so the impurities in the samples should be thoroug...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N1/28G01N30/06
CPCG01N1/28G01N30/06G01N2001/2893
Inventor 朱娴马斌温九平商雪玲马亚新潘琦瑛孙丹陈雯雯楼禹阳郭静
Owner HANGZHOU ZHONGMEI HUADONGPHARMACEUTICAL JIANGDONG CO LTD