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Tetramethylpyrazine extraction and purification method

A technology of tetramethylpyrazine and tetramethylpyrazine dialysate, which is applied in the field of bioengineering to achieve the effects of high impurity removal rate, simple process, and improved product purity and recovery rate

Active Publication Date: 2016-08-17
QILU UNIV OF TECH +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0009] Aiming at the difficulties and defects in the purification of tetramethylpyrazine produced by fermentation, the present invention provides a method for extracting and purifying tetramethylpyrazine

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0042] A method for extracting and purifying tetramethylpyrazine, comprising the following steps:

[0043] (1) After exchanging heat through a tubular heat exchanger, the fermented liquid is heated to 70°C, pumped into a centrifuge by a sanitary centrifugal pump, and centrifuged to separate the bacteria to obtain a supernatant; put the supernatant into a reflux Tube activated carbon decolorization tank, sealed and decolorized for 30 minutes, and maintained at a temperature of 70-80°C; the amount of activated carbon used was 1% of the volume of the supernatant; the pressure during the decolorization process was 0.1-0.12MPa, and the pH was adjusted to 7.0-8.0 after decolorization;

[0044] (2) After filtering the decolorized supernatant of step (1) through a plate and frame filter, it enters a buffer tank, then enters an ultrafiltration system, and after filtering to remove impurities, further removes impurities by nanofiltration to obtain tetramethyl pyrazine dialysate;

[004...

Embodiment 2

[0049] A method for extracting and purifying tetramethylpyrazine, comprising the following steps:

[0050] (1) After exchanging heat through a tubular heat exchanger, the fermentation broth is heated to 80°C, pumped into a centrifuge by a sanitary centrifugal pump, and centrifuged to separate the bacteria to obtain a supernatant; Tube activated carbon decolorization tank, sealed decolorization 40min, maintain temperature 80 ℃; the amount of activated carbon is 1.5% of the volume of the supernatant; the pressure of the decolorization process is 0.12-0.15MPa, after decolorization, adjust the pH to 7.0-8.0;

[0051] (2) After filtering the decolorized supernatant of step (1) through a plate and frame filter, it enters a buffer tank, then enters an ultrafiltration system, and after filtering to remove impurities, further removes impurities by nanofiltration to obtain tetramethyl pyrazine dialysate;

[0052] (3) Concentrate the tetramethylpyrazine dialyzate in step (2) at 70-75° C...

Embodiment 3

[0056] A method for extracting and purifying tetramethylpyrazine, comprising the following steps:

[0057] (1) After exchanging heat through a tubular heat exchanger, the fermented liquid is heated to 75°C, pumped into a centrifuge by a sanitary centrifugal pump, and centrifuged to separate the bacteria to obtain a supernatant; Tube activated carbon decolorization tank, seal decolorization for 20min, maintain the temperature at 75°C; the amount of activated carbon is 1.2% of the volume of the supernatant; the pressure of the decolorization process is 0.15-0.19MPa, and the pH is adjusted to 7.0-8.0 after decolorization;

[0058] (2) After filtering the decolorized supernatant of step (1) through a plate and frame filter, it enters a buffer tank, then enters an ultrafiltration system, and after filtering to remove impurities, further removes impurities by nanofiltration to obtain tetramethyl pyrazine dialysate;

[0059] (3) concentrating the tetramethylpyrazine dialysate in ste...

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Abstract

The invention relates to a tetramethylpyrazine extraction and purification method. The method includes the following steps that firstly, a fermentation solution is heated, thalluses are centrifugally separated to obtain supernatant, and the supernatant is subjected to active carbon decoloration; secondly, the decolorized supernatant is filtered to obtain tetramethylpyrazine dialysate; thirdly, the tetramethylpyrazine dialysate is filtered and then concentrated through a reverse osmosis filter membrane to obtain an infiltration solution; fourthly, the infiltration solution is cooled and crystallized, the temperature is reduced, tetramethylpyrazine crystals are centrifugally separated, then the tetramethylpyrazine crystals are cooled and re-crystallized after redissolving, centrifugal separation is conducted, and high-purity tetramethylpyrazine is obtained. By means of the separation and extraction method, the purity of tetramethylpyrazine is high and is up to 99% or above, and purification efficiency is high and is up to 88% or above.

Description

technical field [0001] The invention belongs to the field of bioengineering, and relates to a method for extracting and purifying tetramethylpyrazine, in particular to a production process for separating and purifying tetramethylpyrazine from fermentation broth. Background technique [0002] Tetramethylpyrazine, molecular formula C 8 h 12 N 2 , molecular weight 136.20, melting point 84-86°C, boiling point 190°C, is a common heterocyclic nitrogen-containing compound, widely exists in food raw materials, processed foods and alcoholic beverages, and is considered to be an important class of aroma compounds with baking Roasted, peanut, hazelnut and cocoa aroma, often used in the deployment of baked goods, cold drinks, meat, dairy products, cigarettes and other flavors. In addition to its use as a food flavor additive, tetramethylpyrazine, as the main active alkaloid component of the rhizome of the Chinese herbal medicine Ligusticum Chuanxiong, has been proven to have pharmaco...

Claims

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Application Information

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IPC IPC(8): C07D241/12
CPCC07D241/12
Inventor 王腾飞孟武王瑞明王建斌
Owner QILU UNIV OF TECH
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