CN101768611B - Method for extracting athomin with mustard seeds as raw material - Google Patents

Method for extracting athomin with mustard seeds as raw material Download PDF

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Publication number
CN101768611B
CN101768611B CN2009102446228A CN200910244622A CN101768611B CN 101768611 B CN101768611 B CN 101768611B CN 2009102446228 A CN2009102446228 A CN 2009102446228A CN 200910244622 A CN200910244622 A CN 200910244622A CN 101768611 B CN101768611 B CN 101768611B
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semen brassicae
brassicae junceae
water
raw material
athomin
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CN101768611A (en
Inventor
郑建秋
李健强
石尚柏
曹永松
卢志军
刘西莉
郑翔
罗来鑫
刘鹏飞
郑炜
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Yunnan Qimin Biological Engineering Co., Ltd.
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BEIJING DAXING MODERN AGRICULTURAL TECHNOLOGY INNOVATION CENTER
Agricultural Hawk's Research Institute Of Modern Agricultural Techniques Of Beijing
China Agricultural University
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Abstract

The invention relates to a method for extracting athomin with mustard seeds as the raw material. The method comprises the following steps: taking mustard seeds in brassica in cruciferae as the processing raw material, soaking the raw material in water after being crushed, and then rapidly and effectively obtaining crude product of athomin by a subcritical water extraction method. Because the subcritical water extraction technology is a novel environment-friendly extraction technology not using or rarely using organic solvent, when being in the subcritical state, water has certain dissolving capacity to semi-polar and non-polar organisms, the polarity, the surface tension and the viscosity of water can be changed by controlling the temperature and the pressure of subcritical water, so that the dissolving capacity of the subcritical water to the organisms can be greatly imoroved, therefore, the extraction efficiency is greatly improved, and the content of allyl isothiocyanate product in athomin is high. Compared with the prior art, the method has the advantages of simple technological line, reasonable technological condition, simple and safe reaction and operation, short reaction time, low solvent loss, low technological cost, and high implementation value and social and economic benefit.

Description

With the Semen Brassicae Junceae is the method that raw material extracts athomin
Technical field
The present invention relates to a kind of is the method that raw material extracts athomin with the Semen Brassicae Junceae.
Background technology
Allyl mustard oil (AITC) is the staple of athomin, can be used as seasonings, storage sanitas, sterilant, sterilant, fine-chemical intermediate and medical treatment product, in industry extensive application such as food, chemical industry, agricultural chemicals and medicine.The method for preparing at present allyl mustard oil mainly contains chemical industry synthesis method and biological extraction method.Biological extraction method Along with people's wherein is to food safety, and the pay attention to day by day of industrial production environment problem makes the biological extraction method that the status of not replacing arranged.
The biological extraction method of allyl mustard oil is to belong to plants such as Semen Brassicae Junceae, horseradish and Euterma Wasabi with the Cruciferae rape for processing raw material; Glucosinolate (Thioglucosides) contained in the raw material is under thioglucose enzyme (Myrosinase) catalysis; Hydrolysis produces lsothiocyanates (ACTI) and glucose (Glucose), and wherein allyl mustard oil (AITC) is acknowledged as mustard oil, wasabi, blue or green mustard is peppery and the main taste compound of leaf mustard goods.Natural mustard oil is good because of its mouthfeel, and advantages such as generally recognized as safe are generally used in people's diet life.Through the document retrieval, " food and machinery " the 4th phase of nineteen ninety 192-201; " Chinese seasonings " 1991 the 4th phases 251; " Chinese seasonings " 2008 the 4th phase 20-24; Patent CN1050896; Reports such as CN02141664.8, the biological extraction technology of athomin plant mainly contains two kinds: a kind of is to adopt liquor principle and equipment, and the mustard seed is pulverized, and stir-fry is mixed, and its essential oil is got in static distillation, blends with vegetables oil, promptly obtains finished product.It is big that but this technology has energy consumption, and productive rate is low, and cost is high, is difficult to form the shortcoming of scale prodn.Another kind is that the mustard seed is pulverized, and sends out system through water, is placed on dynamic steam distillation in the stainless steel cauldron of being with stirring and condensing surface, and overhead product extracts with vegetables oil, is finished product after making with extra care.This method is produced the process length consuming time of allyl mustard oil, and percentage extraction is low, and productive rate is not high yet.
Summary of the invention
The object of the present invention is to provide a kind of easy handling, reaction mechanism is short, and percentage extraction is high, and productive rate is high, green safety, and what the allyl mustard oil product content was high in the athomin is the method that raw material extracts athomin with the Semen Brassicae Junceae.
Of the present invention is the method that raw material extracts athomin with the Semen Brassicae Junceae, comprises the steps:
A, preparation raw material Semen Brassicae Junceae, and with its pulverizing;
B, the Semen Brassicae Junceae after will pulverizing add in the reaction kettle; Soak Semen Brassicae Junceae 1-4 hour after pulverizing with pH 4-6.5, temperature 30-80 ℃ acidic aqueous solution; Adopt prior art that glucosinolate contained in the Semen Brassicae Junceae (Thioglucosides) is hydrolyzed to allyl mustard oil under thioglucose enzyme (Myrosinase) catalysis; Wherein the acid instrumentality of the aqueous solution is an edible acid, and the weight ratio of Semen Brassicae Junceae and water is 1: 2-8, and its hydrolysis equation is following:
Figure G2009102446228D00021
C, utilize prior art Subcritical Water Extraction method, under 1-5Mpa, 100-150 ℃ condition, the material in the reaction kettle is carried out the extraction of 30-60min, the material in the separating reaction still then promptly obtains containing the athomin crude product of allyl mustard oil.
Of the present invention is the method that raw material extracts athomin with the Semen Brassicae Junceae; The Semen Brassicae Junceae raw material is crushed to the 20-40 order in the wherein said steps A; The water that soaks Semen Brassicae Junceae among the said step B is deionized water, and edible acid is acetic acid, lactic acid, oxysuccinic acid, Hydrocerol A, glucono-, tartrate, fumaric acid or xitix, and said acidic aqueous solution soaks Semen Brassicae Junceae 1.5-3 hour after pulverizing; The temperature of acidic aqueous solution is 40-60 ℃, and the weight ratio of said Semen Brassicae Junceae and water is 1: 3-6; Pass through the Subcritical Water Extraction method among the said step C under 1.5-4Mpa, 110-140 ℃ condition, the material in the reaction kettle is carried out 35-60 minute extraction.
Of the present invention is the method that raw material extracts athomin with the Semen Brassicae Junceae, and the acidic aqueous solution among the wherein said step B soaks Semen Brassicae Junceae 1.8-2.5 hour after pulverizing, and the temperature of acidic aqueous solution is 45-55 ℃, and the weight ratio of said Semen Brassicae Junceae and water is 1: 3.5-5; Pass through the Subcritical Water Extraction method among the said step C under 1.8-3Mpa, 115-130 ℃ condition, the material in the reaction kettle is carried out 38-50 minute extraction.
Of the present invention is the method that raw material extracts athomin with the Semen Brassicae Junceae, the Semen Brassicae Junceae after the said acidic aqueous solution immersion among the wherein said step B is pulverized 2 hours, and the temperature of acidic aqueous solution is 50 ℃, the weight ratio of said Semen Brassicae Junceae and water is 1: 4; Among the said step C through the Subcritical Water Extraction method under 2Mpa, 120 ℃ of conditions, the material in the reaction kettle carried out 40 minutes extraction.
Of the present invention is the method that raw material extracts athomin with the Semen Brassicae Junceae; It adopts unique process step; Belong to Semen Brassicae Junceae for processing raw material with the Cruciferae rape,, obtain the athomin bullion quickly and efficiently through the Subcritical Water Extraction method then earlier with being soaked in water after the raw material pulverizing.Because the Subcritical Water Extraction technology is a kind of newer use or few with an organic solvent green abstraction technique; When water is in subcritical state, Semi-polarity and nonpolar organic matter had certain dissolving power, through control to the subcritical water temperature and pressure; Can change polarity, surface tension and the viscosity of water; Make subcritical water increase greatly, and then improve its extraction efficiency greatly that the allyl mustard oil product content is high in the athomin to organic dissolving power.Compared with prior art, method operational path of the present invention is simple, and processing condition are reasonable, and operation is simple and safe; Reaction times is short, and solvent loss is little, and the technology cost is low, yield is high; Producing used extraction agent is water, green economy, and production and use all meet the requirement of national security foodstuff production; Meet current Green Food Industry development trend, make it possess excellent industrial application foreground, have bigger implementary value and economic results in society.Therefore, the method that with the Semen Brassicae Junceae is raw material extracts athomin of the present invention has outstanding substantive distinguishing features and obvious improvement.
Be that the method that raw material extracts athomin is described further with the Semen Brassicae Junceae in the face of the present invention down.
Embodiment
Embodiment 1
Of the present invention is the method that raw material extracts athomin with the Semen Brassicae Junceae, comprises the steps:
A, prepare the raw material Semen Brassicae Junceae, and it is crushed to the 20-40 order;
B, the Semen Brassicae Junceae after will pulverizing add in the reaction kettle; Soak Semen Brassicae Junceae 1-4 hour after pulverizing with pH 4-6.5, temperature 30-80 ℃ acidic aqueous solution; Wherein optimum value is that the temperature of acidic aqueous solution is 50 ℃; Soaked 2 hours; The water that soaks Semen Brassicae Junceae is deionized water preferably; Adopt prior art that glucosinolate contained in the Semen Brassicae Junceae (Thioglucosides) is hydrolyzed to allyl mustard oil under thioglucose enzyme (Myrosinase) catalysis, wherein the acid instrumentality of the aqueous solution is acetic acid or lactic acid or oxysuccinic acid or Hydrocerol A or glucono-or tartrate or fumaric acid or xitix, and the weight ratio of Semen Brassicae Junceae and water is 1: 2 or 1: 2.5 or 1: 3 or 1: 3.5 or 1: 4 or 1: 4.5 or 1: 5 or 1: 5.5 or 1: 6 or 1: 6.5 or 1: 7 or 1: 7.5 or 1: 8; Wherein optimum value is 1: 4, and its hydrolysis equation is following:
Figure G2009102446228D00031
C, utilize prior art Subcritical Water Extraction method, under 1-5Mpa, 100-150 ℃ condition, the material in the reaction kettle is carried out the extraction of 30-60min; Wherein optimum value is under 2Mpa, 120 ℃ of conditions; Material in the reaction kettle is carried out 40 minutes extraction, and the material in the separating reaction still then promptly obtains containing the athomin crude product of allyl mustard oil; Allyl mustard oil content is 66.5% in the product, and oil yield rate is 2.3%.
Embodiment 2
For processing raw material, earlier Semen Brassicae Junceae is ground into the 20-40 order with Semen Brassicae Junceae, adds reaction kettle then; Add deionized water again, the weight ratio of Semen Brassicae Junceae and deionized water is 1: 6, and the potential of hydrogen of using acetic acid to regulate deionized water is pH4.5; And the temperature that makes water is 40 ℃; With this aqueous solution soaking Semen Brassicae Junceae 3 hours, make glucosinolate contained in the Semen Brassicae Junceae (Thioglucosides) under thioglucose enzyme (Myrosinase) catalysis, be hydrolyzed to allyl mustard oil, then through Subcritical Water Extraction method product 50 minutes in the extractive reaction still under 1Mpa, 100 ℃ of conditions; Product in the separating reaction still again; Can obtain the athomin bullion, allyl mustard oil content is 68.6% in the product through detecting, and oil yield rate is 1.9%.
Embodiment 3
For processing raw material, earlier Semen Brassicae Junceae is ground into the 20-40 order with Semen Brassicae Junceae, adds reaction kettle then; Add deionized water again, the weight ratio of Semen Brassicae Junceae and deionized water is 1: 4, and the potential of hydrogen of using Hydrocerol A to regulate deionized water is pH5; And the temperature that makes water is 50 ℃; With this aqueous solution soaking Semen Brassicae Junceae 2 hours, make glucosinolate contained in the raw material (Thioglucosides) under thioglucose enzyme (Myrosinase) catalysis, be hydrolyzed to allyl mustard oil, then through Subcritical Water Extraction method product 40 minutes in the extractive reaction still under 2Mpa, 120 ℃ of conditions; Product in the separating reaction still again; Can obtain the athomin bullion, allyl mustard oil content is 68.2% in the product through detecting, and oil yield rate is 2.2%.
Embodiment 4
For processing raw material, earlier raw material powder is broken into the 20-40 order with Semen Brassicae Junceae, adds reaction kettle then; Add deionized water again, the weight ratio of Semen Brassicae Junceae and deionized water is 1: 2, and the potential of hydrogen of using acetic acid to regulate deionized water is pH6; And the temperature that makes water is 70 ℃; With this aqueous solution soaking Semen Brassicae Junceae 1 hour, make glucosinolate contained in the raw material (Thioglucosides) under thioglucose enzyme (Myrosinase) catalysis, be hydrolyzed to allyl mustard oil, then through Subcritical Water Extraction method product 30 minutes in the extractive reaction still under 5Mpa, 150 ℃ of conditions; Product in the separating reaction still again; Can obtain the athomin bullion, allyl mustard oil content is 66.5% in the product through detecting, and oil yield rate is 2.3%.
Embodiment 5
For processing raw material, earlier raw material powder is broken into the 20-40 order with Semen Brassicae Junceae, adds reaction kettle then; Add deionized water again, the weight ratio of Semen Brassicae Junceae and deionized water is 1: 8, and the potential of hydrogen of using Hydrocerol A to regulate deionized water is pH4; And the temperature that makes water is 60 ℃; With this aqueous solution soaking Semen Brassicae Junceae 4 hours, make glucosinolate contained in the raw material (Thioglucosides) under thioglucose enzyme (Myrosinase) catalysis, be hydrolyzed to allyl mustard oil, then through Subcritical Water Extraction method product 30 minutes in the extractive reaction still under 3Mpa, 140 ℃ of conditions; Product in the separating reaction still again; Can obtain the athomin bullion, allyl mustard oil content is 69.5% in the product through detecting, and oil yield rate is 2.2%.
Semen Brassicae Junceae of the present invention is for processing raw material, and earlier with behind the raw material pulverizing 20-40 order, water is sent out the system hydrolysis, then through the Subcritical Water Extraction method fast, obtain containing the athomin bullion that allyl mustard oil is a staple.Wherein adopting the Subcritical Water Extraction technology, is extraction agent with the water that is in subcritical state, can improve the extraction efficiency of athomin, meets current Green Food Industry development trend, makes it possess excellent industrial application foreground.Compared with prior art, operational path of the present invention is simple, and processing condition are reasonable, and producing used extraction agent is water, green economy, and production and use all meet the requirement of national security foodstuff production.Operation is simple and safe, and the reaction times is short, and solvent loss is little, and the technology cost is low, yield is high, has bigger implementary value and economic results in society.
Embodiment recited above describes preferred implementation of the present invention; Be not that scope of the present invention is limited; Design under the spiritual prerequisite not breaking away from the present invention; Various distortion and improvement that the common engineering technical personnel in this area make technical scheme of the present invention all should fall in the definite protection domain of claims of the present invention.

Claims (4)

1. be the method that raw material extracts athomin with the Semen Brassicae Junceae, it is characterized in that comprising the steps:
A, preparation raw material Semen Brassicae Junceae, and with its pulverizing;
B, the Semen Brassicae Junceae after will pulverizing add in the reaction kettle; Soak Semen Brassicae Junceae 1-4 hour after pulverizing with pH 4-6.5, temperature 30-80 ℃ acidic aqueous solution; Make glucosinolate contained in the Semen Brassicae Junceae (Thioglucosides) under thioglucose enzyme (Myrosinase) catalysis, be hydrolyzed to allyl mustard oil; Wherein the acid instrumentality of the aqueous solution is an edible acid, and the weight ratio of Semen Brassicae Junceae and water is 1: 2-8;
C, utilize the Subcritical Water Extraction method, under 1-5Mpa, 100-150 ℃ condition, the material in the reaction kettle is carried out the extraction of 30-60min, the material in the separating reaction still then promptly obtains containing the athomin crude product of allyl mustard oil.
2. according to claim 1 is the method that raw material extracts athomin with the Semen Brassicae Junceae; It is characterized in that: the Semen Brassicae Junceae raw material is crushed to the 20-40 order in the said steps A; The water that soaks Semen Brassicae Junceae among the said step B is deionized water; Edible acid is acetic acid, lactic acid, oxysuccinic acid, Hydrocerol A, glucono-, tartrate, fumaric acid or xitix; Said acidic aqueous solution soaks Semen Brassicae Junceae 1.5-3 hour after pulverizing, and the temperature of acidic aqueous solution is 40-60 ℃, and the weight ratio of said Semen Brassicae Junceae and water is 1: 3-6; Pass through the Subcritical Water Extraction method among the said step C under 1.5-4Mpa, 110-140 ℃ condition, the material in the reaction kettle is carried out 35-60 minute extraction.
3. according to claim 2 is the method that raw material extracts athomin with the Semen Brassicae Junceae; It is characterized in that: the acidic aqueous solution among the said step B soaks Semen Brassicae Junceae 1.8-2.5 hour after pulverizing; The temperature of acidic aqueous solution is 45-55 ℃, and the weight ratio of said Semen Brassicae Junceae and water is 1: 3.5-5; Pass through the Subcritical Water Extraction method among the said step C under 1.8-3Mpa, 115-130 ℃ condition, the material in the reaction kettle is carried out 38-50 minute extraction.
4. according to claim 3 is the method that raw material extracts athomin with the Semen Brassicae Junceae; It is characterized in that: the Semen Brassicae Junceae after the said acidic aqueous solution immersion among the said step B is pulverized 2 hours; The temperature of acidic aqueous solution is 50 ℃, and the weight ratio of said Semen Brassicae Junceae and water is 1: 4; Among the said step C through the Subcritical Water Extraction method under 2Mpa, 120 ℃ of conditions, the material in the reaction kettle carried out 40 minutes extraction.
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CN102603406B (en) * 2012-03-28 2014-03-19 常熟市润丰农业有限公司 Horseradish soil fertilizer composition for preventing and curing soil-borne disease
CN102746940A (en) * 2012-08-01 2012-10-24 河南华美生物工程有限公司 Method for extracting penoy seed oil by using water
CN103113980B (en) * 2013-02-16 2014-11-05 福建农林大学 Efficient extraction and purification method of mandarin peel oil
CN104621189A (en) * 2014-11-28 2015-05-20 电白县正绿菜业有限公司 Disinfectant containing leaf mustard seed extract
CN107056343A (en) * 2017-04-27 2017-08-18 运嘉(江苏)环保科技有限公司 Subcritical water circular treatment feces of livestock and poultry, dead livestock and poultry, slaughterhouse leftover pieces technique
CN108130192B (en) * 2018-02-28 2021-07-06 浙江舟山彩麟之食品有限公司 Method for extracting high-purity mustard essential oil from mustard seeds
CN113367162A (en) * 2021-05-24 2021-09-10 湖北省烟草公司宜昌市公司 Plant pesticide, preparation and utilization method thereof in tobacco cultivation and preparation
CN113831958A (en) * 2021-11-03 2021-12-24 仲景食品股份有限公司 Method for synchronously extracting mustard essential oil and mustard seed extract

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