Production process for extracting, separating and purifying shikimic acid from cedar needles

Abstract

The invention relates to a production process for extracting, separating and purifying shikimic acid from cedar needles. The process is used for producing shikimic acid by using air-dried fresh cedar needles as raw materials and using industrial alcohol as an extraction solvent for reflux extraction through solvent extraction, silica gel column separation and recrystallization. The method has the characteristics of low cost of raw materials, recycling use of organic solvents in production processes, low production cost, high purity of the obtained product, simple steps, easy popularization, and the like.

Description

technical field

[0001] The invention relates to a production process for extracting, separating and purifying raw material shikimic acid from coniferous plants, in particular to a production process for extracting, separating and purifying shikimic acid from cedar pine needles. Background technique

[0002] Shikimic acid, chemical name 3,4,5-trihydroxy-1-cyclohexene-1-carboxylic acid, molecular formula C 7 h 10 o 5 , molecular weight 174.15. Shikimic acid is an intermediate product of the shikimic acid pathway that widely exists in higher plants and microorganisms. It has anti-tumor and cardiovascular and cerebrovascular effects, and can be used as an anti-avian influenza drug oseltamivir phosphate (trade name Tamiflu) Synthetic raw materials for antitumor drugs such as mycin and glyoxalase inhibitors. In addition, it also plays an important role in biosynthesis, such as phenylpropanoids, aromatic amino acids, flavonoids, etc. are all produced through the shikimate pathw...

Examples

Embodiment 1

[0018] Embodiment 1 The production technology of extracting, separating and purifying shikimic acid from cedar pine needles comprises the following steps:

[0019] (1) Put fresh cedar pine needles in a cool place to dry to obtain dry cedar pine needles.

[0020] (2) the dried cedar pine needles of 3.5kg are placed in the TQ-0.5M produced by Jiangsu Changshu Traditional Chinese Medicine Pharmaceutical Machinery Factory 3 In the multi-functional extraction tank, add industrial ethanol with a mass concentration of 95% according to the liquid-to-material volume ratio of 16:1, and carry out reflux extraction, and extract 3 times in total, and extract 1 hour each time; then filter and merge to obtain the extract and material Slag, slag waste.

[0021] (3) The extract obtained in step (2) is used in the JN type decompression concentration tank produced by Jiangsu Changshu Traditional Chinese Medicine Pharmaceutical Machinery General Factory to carry out decompression recovery of eth...

Embodiment 2

[0027] Embodiment 2 The production technology of extracting, separating and purifying shikimic acid from cedar pine needles comprises the following steps:

[0028] (1) Put fresh cedar pine needles in a cool place to dry to obtain dry cedar pine needles.

[0029] (2) Put 3.5kg dry cedar pine needles in TQ-0.5M 3 In the type multifunctional extraction tank, add mass concentration of 95% industrial ethanol according to the liquid-material volume ratio of 12:1, carry out reflux extraction, extract altogether 3 times, extract 1.5h each time; Then filter, merge, obtain extract and The slag, the slag is discarded.

[0030] (3) The extract obtained in step (2) is reclaimed under reduced pressure using a JN type decompression concentration tank until there is no alcohol smell, and 445 g of fluid extract with a relative density of 1.05 to 1.10 (60° C. thermal measurement) is obtained; Simultaneous recovery Ethanol is processed for reuse.

[0031] (4) Disperse the liquid extract obtai...

Embodiment 3

[0036] Embodiment 3 The production technology of extracting, separating and purifying shikimic acid from cedar pine needles comprises the following steps:

[0037] (1) Put fresh cedar pine needles in a cool place to dry to obtain dry cedar pine needles.

[0038] (2) Put 3.5kg dry cedar pine needles in TQ-0.5M 3 In the type multifunctional extraction tank, add industrial ethanol with a mass concentration of 95% according to the liquid-material volume ratio of 10:1, and carry out reflux extraction, and extract 3 times in total, and extract 1 hour each time; then filter and combine to obtain the extract and material Slag, slag waste.

[0039] (3) The extract obtained in step (2) is reclaimed under reduced pressure using a JN type decompression concentration tank until there is no alcohol smell, and 438g of fluid extract with a relative density of 1.05 to 1.10 (60°C thermal measurement) is obtained; Ethanol is processed for reuse.

[0040] (4) Disperse the liquid extract obtain...

technical field

[0001] The invention relates to a production process for extracting, separating and purifying raw material shikimic acid from coniferous plants, in particular to a production process for extracting, separating and purifying shikimic acid from cedar pine needles. Background technique

[0002] Shikimic acid, chemical name 3,4,5-trihydroxy-1-cyclohexene-1-carboxylic acid, molecular formula C 7 h 10 o 5 , molecular weight 174.15. Shikimic acid is an intermediate product of the shikimic acid pathway that widely exists in higher plants and microorganisms. It has anti-tumor and cardiovascular and cerebrovascular effects, and can be used as an anti-avian influenza drug oseltamivir phosphate (trade name Tamiflu) Synthetic raw materials for antitumor drugs such as mycin and glyoxalase inhibitors. In addition, it also plays an important role in biosynthesis, such as phenylpropanoids, aromatic amino acids, flavonoids, etc. are all produced through the shikimate pathw...

Examples

Embodiment 1

[0018] Embodiment 1 The production technology of extracting, separating and purifying shikimic acid from cedar pine needles comprises the following steps:

[0019] (1) Put fresh cedar pine needles in a cool place to dry to obtain dry cedar pine needles.

[0020] (2) the dried cedar pine needles of 3.5kg are placed in the TQ-0.5M produced by Jiangsu Changshu Traditional Chinese Medicine Pharmaceutical Machinery Factory 3 In the multi-functional extraction tank, add industrial ethanol with a mass concentration of 95% according to the liquid-to-material volume ratio of 16:1, and carry out reflux extraction, and extract 3 times in total, and extract 1 hour each time; then filter and merge to obtain the extract and material Slag, slag waste.

[0021] (3) The extract obtained in step (2) is used in the JN type decompression concentration tank produced by Jiangsu Changshu Traditional Chinese Medicine Pharmaceutical Machinery General Factory to carry out decompression recovery of eth...

Embodiment 2

[0027] Embodiment 2 The production technology of extracting, separating and purifying shikimic acid from cedar pine needles comprises the following steps:

[0028] (1) Put fresh cedar pine needles in a cool place to dry to obtain dry cedar pine needles.

[0029] (2) Put 3.5kg dry cedar pine needles in TQ-0.5M 3 In the type multifunctional extraction tank, add mass concentration of 95% industrial ethanol according to the liquid-material volume ratio of 12:1, carry out reflux extraction, extract altogether 3 times, extract 1.5h each time; Then filter, merge, obtain extract and The slag, the slag is discarded.

[0030] (3) The extract obtained in step (2) is reclaimed under reduced pressure using a JN type decompression concentration tank until there is no alcohol smell, and 445 g of fluid extract with a relative density of 1.05 to 1.10 (60° C. thermal measurement) is obtained; Simultaneous recovery Ethanol is processed for reuse.

[0031] (4) Disperse the liquid extract obtai...

Embodiment 3

[0036] Embodiment 3 The production technology of extracting, separating and purifying shikimic acid from cedar pine needles comprises the following steps:

[0037] (1) Put fresh cedar pine needles in a cool place to dry to obtain dry cedar pine needles.

[0038] (2) Put 3.5kg dry cedar pine needles in TQ-0.5M 3 In the type multifunctional extraction tank, add industrial ethanol with a mass concentration of 95% according to the liquid-material volume ratio of 10:1, and carry out reflux extraction, and extract 3 times in total, and extract 1 hour each time; then filter and combine to obtain the extract and material Slag, slag waste.

[0039] (3) The extract obtained in step (2) is reclaimed under reduced pressure using a JN type decompression concentration tank until there is no alcohol smell, and 438g of fluid extract with a relative density of 1.05 to 1.10 (60°C thermal measurement) is obtained; Ethanol is processed for reuse.

[0040] (4) Disperse the liquid extract obtain...