CN102492739A - New technology for preparing natural acetic acid 3-methylthio proply ester spice and ester spice thereof - Google Patents
New technology for preparing natural acetic acid 3-methylthio proply ester spice and ester spice thereof Download PDFInfo
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- CN102492739A CN102492739A CN2011104190410A CN201110419041A CN102492739A CN 102492739 A CN102492739 A CN 102492739A CN 2011104190410 A CN2011104190410 A CN 2011104190410A CN 201110419041 A CN201110419041 A CN 201110419041A CN 102492739 A CN102492739 A CN 102492739A
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Abstract
The invention relates to a new technology for preparing a natural acetic acid 3-methylthio proply ester spice and an ester spice product thereof, and relates to a new technology for preparing a natural ester spice by converting 3-methylthio propanol and acetic acid which serve as main raw materials by an enzyme method under the nonaqueous phase condition. According to the technology, acetic acid 3-methylthio proply ester (EMTP) has strong pineapple fragrance, is a spice for blending multiple fruity essences, meaty essences and wine essences and is widely applied in industry of drinks, jam, candies, baked food, medicines, daily chemicals and the like. According to the technology, a nonaqueous phase enzymatic conversion technology and an ultrasonic field (non-ultrasonic field) reinforcement technology are integrated, the 3-methylthio propanol and the acetic acid which are used for fermentation are used as main raw materials, and the natural acetic acid 3-methylthio proply ester spice is prepared by utilizing the nonaqueous phase conversion of lipase. According to the technology, the reaction condition is mild, the defects of high energy consumption and serious pollution in the chemical synthesis of the 3-methylthio proply ester are overcome, the naturalness and edible safety of the ester spice are enhanced, and the additional value and benefit of the ester spice are improved.
Description
Technical field:
The invention belongs to Food Science and Engineering, technical field of biochemical industry; Relating to 3 methylthiol propyl alcohol, acetate is main raw material; As catalyzer, enzymatic conversion method prepares the new technology and the gained natural esters spice product thereof of acetate 3-methylthio group propyl ester spices under nonaqueous phase, ultrasonic field reinforcement or non-ultrasonic field conditions with lypase.
Background technology:
3 methylthiol propyl alcohol (Methionol; Have another name called pineapple alcohol) be the characteristic perfumery matter of China's distilled spirit with sesame flavour; Also be the important aroma component of multiple leavened foods such as wine, beer, yellow rice wine, soy sauce, beans sauce, cheese, bacon, its fragrance threshold value is low, and the suggestion consumption is 0.1～10mg/kg in food; Its local flavor presents Fructus Hordei Germinatus fragrance, sesame oil flavor and mellow soil beans flavor successively, and its FEMA is numbered 3415.Acetate 3-methylthio group propyl ester (Ethyl-3-methyl-thiopropionate; EMTP) also be a kind of important sulfur-bearing spices; Has strong pineapple typical flavor; Its FEMA is numbered 3343, and EMTP is allotment pineapple, oranges and tangerines, horseradish, tomato, onion, pork, beef, chicken, chocolate, the wine conventional perfumes with multiple essence such as essence.
At present the main working method of acetate 3-methylthio group propyl ester is to be main raw material with 3 methylthiol propyl alcohol and acetic anhydride, and the sulphuric acid catalysis esterification prepares.This method is easy and simple to handle, but the vitriol oil is serious to equipment corrosion, and environmental pollution is serious, and the preparation Ester do not have natural sex, its preparation essence and flavoring agent application receive certain limitation, price is low.
The integrated nonaqueous phase enzyme-catalyzed change technology of the present invention, ultrasonic field intensifying technology are main raw material with fermentation 3 methylthiol propyl alcohol and acetate, preparation Natural ester spices.Reaction conditions is gentle, meets the social desirability of environmentally friendly production, and has strengthened the natural sex and the edible safety of ester perfume product.
Summary of the invention:
The invention provides a kind of new preparation technology and ester spice product thereof that is suitable for natural acetate 3-methylthio group propyl ester spices; This technology is to utilize pretreated fermentation 3 methylthiol propyl alcohol and acetate to be main raw material; With lypase is catalyzer; Adopt non-aqueous system, assisting ultrasonic field intensity or non-ultrasonic field intensity technology transform new technology of the natural acetate 3-methylthio group propyl ester spices of preparation and products thereof.
Technical scheme of the present invention:
Technology such as the integrated nonaqueous phase enzyme-catalyzed change of the present invention, ultrasonic field reinforcement preparation Natural ester spices.At first need raw material 3 methylthiol propyl alcohol, acetate are dewatered in advance, decolour, prevent reversible reaction and lypase inactivation, improve nonaqueous phase enzymatic reaction effect; The adding of acetate intermittent type prevents the influence of excess acid to lipase activity; Add molecular sieve absorbing and removing water generation reaction, promote esterification to carry out; The ultrasonic field intensity of auxiliary suitable intensity is strengthened enzymatic reaction and is carried out, and shortens the reaction times, improves feed stock conversion; Rectifying shunting or absorption--resolve and obtain highly purified natural acetate 3-methylthio group propyl ester spice product.
Technique effect of the present invention:
The invention provides a kind of new preparation technology and ester spice product thereof that is suitable for natural acetate 3-methylthio group propyl ester spices; This techniques make use fermentation 3 methylthiol propyl alcohol and acetate are main raw material; Reaction conditions is gentle; Feed stock conversion is high, meets the requirement that environmental friendliness is produced, and gained ester perfume product has natural sex and edible safety preferably.
Add conditions such as sour number of times, temperature, molecular sieve, lypase through control proportioning raw materials, intermittent type, at solvent-free system, shaking table reaction 5h～60h, or auxilliaryly add ultrasonic field intensity reaction 0.5h～25h, the productive rate of acetate 3-methylthio group propyl ester reaches 50%～70%.
Embodiment:
Raw material 3 methylthiol propyl alcohol, acetate are dewatered in advance, decolour; In solvent-free system, add respectively 3 methylthiol propyl alcohol and acetate [3 methylthiol propyl alcohol: acetate=(1～6): 1 (V/V), acetate divides 1～10 adding; Each 1～5 hour at interval]; Immobilized lipase 0.03%～8% (W/V), molecular sieve 0.3%～15% (W/V) is 15～60 ℃ of temperature; Shaking speed 20～250r/min carries out the reaction of 5h～60h; Or the auxilliary frequency 5～150kHz, power 0.1～10W/cm of adding
2Ultrasonic field intensity is carried out 0.5h～25h reaction, and timing sampling GC-MS detects feed stock conversion, purpose efficiency of pcr product, accomplishes the nonaqueous phase Enzymatic transformation preparation of acetate 3-methylthio group propyl ester spices.
Claims (4)
1. a new preparation technology and ester spice product thereof that is suitable for natural acetate 3-methylthio group propyl ester spices; It is characterized in that with 3 methylthiol propyl alcohol and acetate be main raw material; With lypase is catalyzer; At solvent-free non-aqueous system, strengthen the assisting ultrasonic field or non-ultrasonic field is strengthened enzymatic reaction, transforms the technology and the ester product thereof of the natural acetate 3-methylthio group propyl ester spices of preparation.
2. a kind of new preparation technology and ester spice product thereof that is suitable for natural acetate 3-methylthio group propyl ester spices according to claim 1; It is characterized in that raw material 3 methylthiol propyl alcohol and acetate have good natural sex; 3 methylthiol propyl alcohol is the product of fermentation L-methionine(Met) (methionine(Met)) and cereal glucide, and acetate is fermented cereal glucide gained acetate.
3. a kind of new preparation technology and ester spice product thereof that is suitable for natural acetate 3-methylthio group propyl ester spices according to claim 1; It is characterized in that solvent-free non-aqueous system; With lypase is catalyzer; Assisting ultrasonic field intensity or non-ultrasonic field intensity are carried out the esterification of 3 methylthiol propyl alcohol and acetate, transform the Natural ester spices of preparation.
4. a new preparation technology and an ester spice product thereof that is suitable for natural acetate 3-methylthio group propyl ester spices dewaters raw material 3 methylthiol propyl alcohol, acetate in advance, decolours; In solvent-free system, add respectively 3 methylthiol propyl alcohol and acetate [3 methylthiol propyl alcohol: acetate=(1～6): 1 (V/V), acetate divides 1～10 adding; Each 1～5h at interval (hour)]; Immobilized lipase 0.03%～8% (W/V), molecular sieve 0.3%～15% (W/V) is 15～60 ℃ of temperature; Shaking speed 20～250r/min carries out the reaction of 5h～60h; Or auxilliary frequency 5～150kHz, the power 0.1～10W/cm of adding
2Ultrasonic field is strengthened, and carries out the reaction of 0.5h～25h, accomplishes the acetate 3-methylthio group propyl ester spice product of nonaqueous phase Enzymatic transformation new preparation technology and preparation thereof.
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| Application Number | Priority Date | Filing Date | Title |
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| CN2011104190410A CN102492739A (en) | 2011-12-15 | 2011-12-15 | New technology for preparing natural acetic acid 3-methylthio proply ester spice and ester spice thereof |
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| CN2011104190410A CN102492739A (en) | 2011-12-15 | 2011-12-15 | New technology for preparing natural acetic acid 3-methylthio proply ester spice and ester spice thereof |
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| CN102492739A true CN102492739A (en) | 2012-06-13 |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103598489A (en) * | 2013-12-04 | 2014-02-26 | 中国热带农业科学院南亚热带作物研究所 | Method for improving content of aroma components in pineapple fruits |
| CN106616835A (en) * | 2017-03-02 | 2017-05-10 | 山东天博食品配料有限公司 | Purple sweet potato essence and preparation method thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1594585A (en) * | 2004-06-25 | 2005-03-16 | 河北工业大学 | Process for enzymatic synthesis of ethyl lactate in solvent phase |
| CN102492738A (en) * | 2011-12-08 | 2012-06-13 | 北京工商大学 | Novel technology for preparing natural ethyl-3-methyl-thiopropionate spice and ester spice prepared by novel technology |
-
2011
- 2011-12-15 CN CN2011104190410A patent/CN102492739A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1594585A (en) * | 2004-06-25 | 2005-03-16 | 河北工业大学 | Process for enzymatic synthesis of ethyl lactate in solvent phase |
| CN102492738A (en) * | 2011-12-08 | 2012-06-13 | 北京工商大学 | Novel technology for preparing natural ethyl-3-methyl-thiopropionate spice and ester spice prepared by novel technology |
Non-Patent Citations (2)
| Title |
|---|
| 《食品工业科技》 20111031 温明显 等 "正己烷反应体系中酶法转化乙酸3-甲硫基丙醇酯的工艺条件" 第212-214页 1-4 , 第10期 * |
| 温明显 等: ""正己烷反应体系中酶法转化乙酸3-甲硫基丙醇酯的工艺条件"", 《食品工业科技》 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103598489A (en) * | 2013-12-04 | 2014-02-26 | 中国热带农业科学院南亚热带作物研究所 | Method for improving content of aroma components in pineapple fruits |
| CN103598489B (en) * | 2013-12-04 | 2015-01-14 | 中国热带农业科学院南亚热带作物研究所 | Method for improving content of aroma components in pineapple fruits |
| CN106616835A (en) * | 2017-03-02 | 2017-05-10 | 山东天博食品配料有限公司 | Purple sweet potato essence and preparation method thereof |
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Application publication date: 20120613 |