CN105176685A - Method for preparing natural aroma-enhanced orange essential oil with enzymatic method - Google Patents
Method for preparing natural aroma-enhanced orange essential oil with enzymatic method Download PDFInfo
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Abstract
The invention discloses a method for preparing natural aroma-enhanced orange essential oil with an enzymatic method. The method comprises steps as follows: lipase is added to orange essential oil to react at the temperature of 35-60 DEG C for 4-24 h under the condition of 100-300 RPM, solid lipase is removed through filtration, and the natural aroma-enhanced orange essential oil is obtained, wherein 0.01-0.05 g of the lipase is added to every milliliter of the orange essential oil. Single alcohols and acids in the orange essential oil react to produce aromatic ester under the catalysis of the lipase, or a natural essence component is biologically synthesized or decomposed through an enzymatic reaction, purely natural essential oil with the special aroma is produced or the content of aromatic substances in the purely natural essential oil is increased, so that the top note, the aroma concentration and the aroma type of the existing orange essence are enhanced and improved. With the adoption of the method, the aroma performance and the essence quality of the orange essential oil can be substantially improved, besides, aroma types in different styles can be obtained through addition of different natural acids and alcohols, the product has various styles, and meanwhile, the method is simple and efficient.
Description
Technical field
The present invention relates to a kind of enzymatic preparation method of natural flavouring tangerine oil, particularly a kind of lipase enzymatic production pure natural tangerine oil and realize tangerine oil flavouring.
Background technology
Perfume material needed for current domestic food flavour production, major part is still chemosynthesis.Due to the impact of the factor such as production technique, appointed condition, usually there is the fluctuation of quality unstable in chemically composite perfume, objectionable impurities remains phenomenons such as exceeding standard, thus affects the security of food flavour and even food.Along with compatriots strengthen day by day to the attention of food safety, the demand of natural essence product is also maked rapid progress, rapid development.But domestic natural or class natural essence product is still in the blank stage, this field is badly in need of filling up.
Tangerine oil is (the accounting for 2%) left and right of extracting from the pericarp of Citrus Plants.One of staple commodities important in spice oil.Tangerine oil has delicate sweet taste, except the peel of Citrus reticulata Blanco taste of uniqueness, has also been with a little faint fragrance of a flower.The pure and fresh smell of tangerine oil has the effect improving spirit, is usually used in flatly holding up dejected and anxiety.It is had many uses, and as made the spices of beverage, biscuit, cake, candy, chewing gum etc., also can be used as perfume, makeup, the spices of soap etc., and part can be done medicinal, is indispensable a kind of volatile oil in foods and cosmetics industry.
The extracting method such as steam distillation, solvent-extraction process, supercritical extraction, milling process mainly can be used from citrus peel to extract tangerine oil at present.Wherein, cold grinding method and cold-press are except fuel-displaced mode is different, and follow-up operation is substantially identical; Solvent extration is different according to selected solvent, the quality differential of extraction oil is larger, conventional extraction solvent has normal hexane, sherwood oil, Virahol, ethyl acetate etc., because solvent extraction is easy to the materials such as the pigment in peel of Citrus reticulata Blanco, flavonoid to extract together, cause the later separation purification ratio of essential oil more difficult; Supercritical fluid extraction mainly adopts supercritical carbon dioxide fluid to extract, although the essential oil quality obtained is better, facility investment is too large, and operational condition requires higher.Also must be pointed out, it is strong not to there is fragrance in the tangerine oil of extracting directly, and fragrance is single, solvent residues, and is applied to finished product such as beverage etc. and easily produces the problem such as oil slick and deterioration.
Application number has been that 200810043530.9 Chinese invention patent applications disclose (publication number CN101608143A) a kind of citrus flavor preparation method (Chang Gu river spices (Shanghai) Co., Ltd.), its preparation method comprises the steps: 1) essential oil of citrus is mixed with aqueous ethanolic solution, then be cooled to 10 ~ 20 DEG C, left standstill 1 ~ 2 month; 2) by step 1) product that obtains adopts the method for temperature programming, and be heated to 25 ~ 30 DEG C, the speed of described temperature programming is 1 ~ 2 DEG C/day; 3) then by step 2) product adopt the method for programmed cooling, be cooled to 10 ~ 20 DEG C, the speed of described programmed cooling is 1 ~ 2 DEG C/day; 4) by step 3) product filter, underpressure distillation, flings to aqueous ethanolic solution, namely obtains the citrus essential oil after purifying, namely can be citrus flavor.After the method tangerine oil mixes with ethanolic soln, need cooling to leave standstill 1 ~ 2 month, then product adopts program falling-rising temperature and filters, underpressure distillation, and the citrus essential oil obtained after purifying is citrus flavor.The method length consuming time (1 ~ 2 month), production efficiency is low, is unsuitable for scale operation.
Summary of the invention
The object of the invention is the deficiency overcoming prior art existence, provides a kind of with short production cycle, has natural characteristic, can prepare the enzymatic method preparation method of the natural flavouring tangerine oil of different flavor style.
The present invention can fill up the vacancy of the preparation of current tangerine oil and flavouring research, especially utilizes enzyme process enzymatic reaction to realize the preparation of natural citrus essential oil and flavouring.Pass through enzymatic reaction, fragrance, the odor type performance of tangerine oil obtain and significantly improve and enrich, simultaneously by adding different alcohol, and different acid and the collocation of different acid alcohols, different aromas feature, different flavor style can be prepared, stable tangerine oil product best in quality and essence.Especially the acid added and alcohol are that microorganism can fermentative production, then have more natural characteristic by flavouring tangerine oil prepared by green enzyme process, meet the standard of " all-natural product " rank of European Union.Natural flavouring tangerine oil prepared by the present invention can be used for the essence of composite different aromas style, also can directly apply to foodstuffs industry and chemical engineering industry as natural essence.
The object of the invention is achieved through the following technical solutions:
A kind of enzymatic method preparation method of natural flavouring tangerine oil: added by lipase in tangerine oil, 35 ~ 60 DEG C, under 100 ~ 300RPM condition, reacts 4 ~ 24 hours, solids removed by filtration lipase, obtains natural flavouring tangerine oil; Every milliliter of tangerine oil adds the amount 0.01 ~ 0.05 gram of lipase.
For realizing the object of the invention further, preferably, described lipase is added in tangerine oil also to comprise add alcohol; The amount of the alcohol added is 0.5 ~ 5.0% of tangerine oil volume.
Preferably, lipase is added in tangerine oil and alcohols also to comprise and add acid; The acid added and the mol ratio of alcohol are 1:1 ~ 1:5.
Preferably, described lipase is the lipase with esterification function; In reaction system, the enzyme work of every gram of lipase is higher than 400U.
Preferably, described alcohol be fermentable produce ethanol, lemongrass or Geraniol.
Preferably, described acid is the natural acids of microorganism by fermentative production.Preferably, described natural acids is one or more in caproic acid, acetic acid, butyric acid and capric acid.
Relative to prior art, tool of the present invention has the following advantages:
1) the present invention can make the script in tangerine oil fragrance obviously not contributed to the acid and alcohol that even produce unhappy smell by adding lipase, changes into the ester with peculiar fragrance feature.By adding lipase and ethanol, making in tangerine oil, not contribute the composition of fragrance and ethanol under the catalysis of lipase, producing and be easy to volatilize, the aromatic ethyl ester of tool.Or by adding geraniol and lipase, the content of the citronellyl acrylate fragrance of orange essential oil being had to significant contribution can be increased.Can the acid alcohol of fermentative production by adding microorganism, corresponding ester is produced under the effect of lipase, such as there is clever clearly strong hesperidium fragrant, have pineapple, banana, apple breath ethyl butyrate, have Qu Xiang, pineapple odor type fragrance ethyl hexanoate, have cognac fragrance ethyl octylate, there is rose fragrance, again there is fruit, the butyric acid leaf-alcohol ester etc. of banana and grape fragrance.By the generation of these characteristic perfume esters, can prepare and have that different characteristics fragrance, odor type are abundant, colory natural flavouring tangerine oil.Meanwhile, also by adding acid and the alcohol of mixing, compound natural flavouring tangerine oil can be prepared.
2) the present invention prepares natural citrus essence by zymotechnic enzymatic reaction or to its flavouring, the tangerine oil fragrance not only solving extraction is single, the shortcoming that fragrance is strong not, quality is lower, simultaneously production efficiency comparatively prior art significantly improve, only need 4 ~ 24h to realize quality-improving.
3) the present invention in case of need, adds natural acid alcohol in tangerine oil while introducing lipase, can generate the natural fruity flavor of corresponding odour characteristics, to enrich the fragrance of tangerine oil, promotes the quality of citrus flavouring.If introducing acid or alcohol are natural in production process, pure natural or closely natural essence more can be prepared.
4) the present invention reclaims immobilized enzyme by simple solid-liquid separation and can obtain natural flavouring tangerine oil.And lipase can reuse.
5) the present invention can increase substantially fragrance performance, the essence quality of tangerine oil, and can obtain the odor type of different-style by adding different natural acid alcohols, and make the richer change of product style, while method is simply efficient.
6) the natural flavouring tangerine oil that prepared by the present invention can be used for the essence of composite different aromas style, also can directly apply to foodstuffs industry and chemical engineering industry as natural essence.
Accompanying drawing illustrates:
Fig. 1 be sweet orange oil add ethanol enzymatic (embodiment 3, product 3) first half GC ?the total ion figure of MS.
Fig. 2 be sweet orange oil add ethanol enzymatic (embodiment 3, product 3) latter half GC ?the total ion figure of MS.
Fig. 3 be orange essential oil add ethanol enzymatic (embodiment 4, product 5) first half GC ?the total ion figure of MS.
Fig. 4 be orange essential oil add ethanol enzymatic (embodiment 4, product 5) latter half GC ?the total ion figure of MS.
Embodiment
The following examples will be further explained the present invention, but the present invention is not limited only to these embodiments, the scope that these embodiments do not limit the present invention in any way.
In the embodiment of the present invention GC ?MS detection method as follows: adopt two-stage method to detect the composition of tangerine oil.
Sample pretreatment: filter the flavouring oranges and tangerines that obtain and to be placed in ground shaking flask 3 days, get 5 μ l afterwards in the HPLC normal hexane of 995 μ l.
1) GC ?MS species analysis condition (first half section)
Instrument: AgilentTechnologies7890A gas chromatograph/AgilentTechnologies5975C mass spectrograph;
Chromatographic column: 5% phenyl methyl silicon oxide capillary column, HP ?5MS, 30m × 250 μm × 0.25 μm;
Injector temperature: 250 DEG C;
Temperature programming: initial temperature 40 DEG C, keeps 4 minutes, is then raised to 76 DEG C with 3 DEG C of min and keeps 0 minute, rear operating temperature 280 DEG C;
Mass Spectrometry Conditions: carrier gas is high-purity helium, flow 1mL/min; Ion source: EI source; Ion source temperature: 230 DEG C; Quadrupole temperature: 150 DEG C; Electron energy 70eV; Solvent delay 3.00 minutes; Sweep limit 30 ~ 200u.
2) GC ?MS species analysis condition (second half section)
Instrument: AgilentTechnologies7890A gas chromatograph/AgilentTechnologies5975C mass spectrograph;
Chromatographic column: 5% phenyl methyl silicon oxide capillary column, HP ?5MS, 30m × 250 μm × 0.25 μm;
Injector temperature: 250 DEG C
Temperature programming: initial temperature 40 DEG C, keeps 4 minutes, is then raised to 82 DEG C with 3 DEG C of min and keeps 0 minute, is then raised to 280 DEG C with 10 DEG C/min and keeps 0 minute.
Mass Spectrometry Conditions: carrier gas is high-purity helium, flow 1mL/min; Ion source: EI source; Ion source temperature: 230 DEG C; Quadrupole temperature: 150 DEG C; Electron energy 70eV; Solvent delay 18.00 minutes; Sweep limit 30 ~ 200u.
Embodiment 1
(by Guangzhou, Zhen Yun spices company limited provides to measure sweet orange oil with graduated cylinder, Brazil's single times of sweet orange oil) 20mL is in 50mL tool plug port grinding bottle, in tool plug port grinding bottle, adding lipase PCALB again, (prepared by Chinese invention patent ZL200910039860.5 embodiment 4 method, enzyme is lived as 412U/g) 0.4g, then tool plug port grinding bottle is placed in constant-temperature table, at 45 DEG C, under 200r/min condition, carry out enzymatic reaction, 12h termination reaction.Filter and remove lipase, the sweet orange oil room temperature after filtration is placed and within 3 days, can be obtained stable pure natural flavouring sweet orange oil, called after product 1.
Sample pretreating method and GC ?MS detection method are as introduced in embodiment.Product 1 and former state contrast newly-increased compound and account for always measures material degree (increase newly compound GC ?MS peak area ratio all substances GC ?MS peak area) as follows: anti-Shi ?2,8 ?Shuan Huan ?p ?peppermint (6.874%), lauryl aldehyde (1.47%), sad ester in the last of the ten Heavenly stems (1.852%), propylthio sulfonic acid tridecyl ester (4.699%).The ratio that oxygenatedchemicals accounts for detectable substance reduces 6.391%.The ratio that the Karvon main component of unpleasant odor (in the tangerine oil) accounts for detectable substance reduces 8.64%.
Can be found out by the data of GC ?MS, increased that lauryl aldehyde has soap perfume (or spice), wax is fragrant, aldehyde is fragrant, oranges and tangerines are fragrant and the violet fragrance of a flower newly, the Content of Carvone simultaneously with unhappy smell reduces 8.64%.Improve the fragrance characteristic of sweet orange oil.
Embodiment 2
(by Guangzhou, Zhen Yun spices company limited provides to measure orange essential oil with graduated cylinder, cold press mandarin oil) 20mL is in 50mL tool plug port grinding bottle, in tool plug port grinding bottle, adding lipase PCALB again, (prepared by Chinese invention patent ZL200910039860.5 embodiment 4 method, enzyme is lived as 412U/g) 0.4g, then tool plug port grinding bottle is placed in constant-temperature table, at 45 DEG C, under 200r/min condition, carry out enzymatic reaction, 12h termination reaction.Filter and remove lipase, the orange essential oil room temperature after filtration is placed and within 3 days, can be obtained stable pure natural flavouring orange essential oil, called after product 2.
Sample pretreating method and GC ?MS detection method are as introduced in embodiment.Contrast newly-increased compound with former state and account for the degree (account form is as embodiment 1) always measuring material as follows: n-decyl decylate (0.341%).
Embodiment 3
(by Guangzhou, Zhen Yun spices company limited provides to measure sweet orange oil with graduated cylinder, Brazil's single times of sweet orange oil) 20mL is in 50mL tool plug port grinding bottle, in tool plug port grinding bottle, adding lipase PCALB more respectively, (lipase added respectively is prepared by patent ZL200910039860.5 embodiment 4 method, and enzyme is lived as 412U/g; Commercial lipases Novzyme435, Novozymes Company, production code member: 43101M), lipase consumption is 0.2g, and dehydrated alcohol 500 μ l, then tool plug port grinding bottle is placed in constant-temperature table, at 50 DEG C, under 250r/min condition, carry out enzymatic reaction, 12h termination reaction.Filter and remove lipase, the sweet orange oil room temperature after filtration is placed and within 3 days, can be obtained stable pure natural flavouring sweet orange oil; The product that the product called after product 3, Novzyme435 that PCALB obtains obtains is product 4.
Sample pretreating method and GC ?MS detection method as embodiment introduction.Product 3 and each composition of former state contrast (as shown in table 1 below) GC ?the total ion maps of MS see Fig. 1 and Fig. 2.
Table 1 sweet orange oil adds each composition transfer statistics of ethanol enzymatic 24h (embodiment 3, product 3)
Note: a: adopt gas chromatography mass spectrometry (GC ?MS) to detect component and the content of sweet orange oil before and after enzymatic.
B: with each component GC of control group sweet orange oil of not enzyme-added and ethanol ?the peak area of MS for 100%.The each component GC of the sweet orange oil of enzymatic after 24 hours ?the peak area of MS be relative percentage.
Wherein ↑: the per-cent that after representing enzymatic, material peak area increases.
↓: the per-cent that after representing enzymatic, material peak area reduces.
Do not detect in ↑ 100 these material control group sweet orange oils of expression, can detect after enzymatic.
↓ 100 represent in this material control group sweet orange oil and can detect, and can detect out after enzymatic.
Product fragrance is evaluated:
After product 3 and the former state room temperature of sweet orange oil are placed 3 days, sample presentation please the fragrant slip-stick artist of product be evaluated.
Slip-stick artist evaluates: the fragrance of product 3 fragrance and former state is variant, is mainly reflected in the fragrant aspect of head.
Compound can be increased newly from table 1 and account for the degree (account form is as embodiment 1) always measuring material as follows: trans-2,8-dicyclo-p-peppermint (5.686%), ethyl octylate (3.192%, cognac fragrance), lauryl aldehyde (1.264%), ethyl decylate (1.590%), ethyl undecanoate (0.327%), alkanoic acid ethyl ester (1.464%).The ratio that oxygenatedchemicals accounts for detectable substance reduces 5.062%.But the ratio that Karvon accounts for detectable substance reduces 8.795%.The ratio that limonene oxide accounts for detectable substance reduces 1.885%.Newly-increased compound all has obvious fragrance characteristic, volatile compounds.The Karvon overall proportion simultaneously with pungent gas and cold air reduces.Therefore the odour characteristics of sweet orange oil can be made obviously to improve, especially initial fragrance impression and head perfume.Also the evaluation result of teacher fragrant with product conforms to.
The product that Novzyme435 obtains is product 4, increase compound newly and account for the degree (account form is as embodiment 1) always measuring material as follows: trans-2,8-dicyclo-p-peppermint (4.745%), ethyl octylate (2.636%, cognac fragrance), lauryl aldehyde (0.964%), ethyl decylate (1.332%), ethyl undecanoate (0.288%), alkanoic acid ethyl ester (1.446%).
Application number has been still can keep pure and fresh pleasant spy aromatic citrus essential oil sweetener after 201310080691.6 Chinese invention patent applications disclose (publication number CN103113990A) a kind of dilution.It increases the fragrance level of citrus essential oil by adding natural eucalyptus quintessence oil, allyl oenanthate, acetic acid Soviet Union and fragrant ester, octanal, citral, Terpineol 350, phantol etc., thus reaches the object of flavouring.This application be add in citrus essential oil mass percent 5% ?10% citrus essential oil sweetener.The sweetener price of adding is more expensive, and simultaneously each monomer adds separately and easily causes fragrance impure, and can not adjust for different tangerine oils.The present embodiment 3 is by adding dehydrated alcohol and zymin thus reaching the object of citrus essential oil flavouring, not only low price, and zymin can be reused, different flavoring substances can be produced according to different tangerine oils, obtained flavouring tangerine oil fragrance all with.
Embodiment 4
Orange essential oil (Zhen Yun spices company limited provides by Guangzhou) 20mL is measured in 50mL tool plug port grinding bottle with graduated cylinder, in tool plug port grinding bottle, adding lipase PCALB more respectively, (lipase added respectively is prepared by Chinese invention patent ZL200910039860.5 embodiment 4 method, and enzyme is lived as 412U/g; Commercial lipases Novzyme435, Novozymes Company, production code member: 43101M), lipase consumption is 0.2g, and dehydrated alcohol 500 μ l, is then placed in constant-temperature table tool plug port grinding bottle, at 50 DEG C, under 250r/min condition, carry out enzymatic reaction, 12h termination reaction.Filter and remove lipase, the orange essential oil room temperature after filtration is placed and within 3 days, can be obtained stable pure natural flavouring orange essential oil, the product called after product 5 that PCALB is obtained.The product that Novzyme435 obtains is product 6.
Sample pretreating method and GC ?MS detection method are as introduced in tool embodiment.Product 5 and former state contrast as shown in table 2, GC ?the total ion maps of MS see Fig. 3, Fig. 4.
After table 2 orange essential oil enzymatic 24h, the composition transfer of (product 5) is added up
Note a: adopt gas chromatography mass spectrometry (GC ?MS) to detect component and the content of sweet orange oil before and after enzymatic.
B: with each component GC of control group orange essential oil of not enzyme-added and ethanol ?the peak area of MS for 100%.The orange essential oil each component GC of enzymatic after 24 hours ?the peak area of MS be relative percentage.
Wherein ↑: the per-cent that after representing enzymatic, material peak area increases.
↓: the per-cent that after representing enzymatic, material peak area reduces.
Do not detect in ↑ 100 these material control group sweet orange oils of expression, can detect after enzymatic.
↓ 100 represent in this material control group sweet orange oil and can detect, and can detect out after enzymatic.
After product 5 and the former state room temperature of orange essential oil are placed 3 days, sample presentation please the fragrant slip-stick artist of product be evaluated.
Product fragrant teacher evaluate: the fragrance of product 4 is variant with the fragrance of former state, is mainly reflected in head perfume aspect.Wherein product 4 is more obvious compared with the change of orange essential oil former state.
As shown in Table 2, increase compound newly and account for the degree always measuring material as follows: ethyl octylate (1.335%), ethyl decylate (0.702%), alkanoic acid ethyl ester (0.609%), ethyl pelargonate (0.218%).Newly-increased compound is all volatile, has diffusible fatty-acid ethyl ester, and has fruit character fragrance, obviously can improve the odour characteristics of orange essential oil.Especially initial fragrance impression and head perfume.Also the evaluation result of teacher fragrant with product conforms to.
The product that Novzyme435 obtains is product 6, increase compound newly and account for the degree (account form is as embodiment 1) always measuring material as follows: ethyl octylate (1.462%, cognac fragrance), ethyl pelargonate (0.345%) ethyl decylate (0.723%), ethyl undecanoate (0.345%), alkanoic acid ethyl ester (1.621%).
Embodiment 5
Sweet orange oil (Zhen Yun spices company limited provides by Guangzhou) 20mL is measured in 50mL tool plug port grinding bottle with graduated cylinder, in tool plug port grinding bottle, adding lipase PCALB again, (prepared by Chinese invention patent ZL200910039860.5 embodiment 4 method, enzyme is lived as 2000U/g) butyric acid of 0.2g and 420 μ l, the acetic acid of 52 μ l, the caproic acid of 52 μ l, the leaf-alcohol of 50 μ l, the dehydrated alcohol of 450 μ l, then tool plug port grinding bottle is placed in constant-temperature table, at 55 DEG C, enzymatic reaction is carried out, 12h termination reaction under 250r/min condition.Filter and remove lipase, the sweet orange oil room temperature after filtration is placed and within 3 days, can be obtained stable pure natural flavouring sweet orange oil, called after product 7.
After product 7 and sweet orange oil former state room temperature are placed 3 days, sample presentation please the fragrant slip-stick artist of product be evaluated.
Product fragrant teacher evaluate: the fragrance of product 7 has obvious change compared with the fragrance of former state sweet orange oil, and in product 7, the fragrance of ethyl butyrate, ethyl hexanoate all can obviously embody.
Sample pretreating method and GC ?MS detection method as shown in the specific embodiments.GC ?MS detect find ethyl butyrate, ethyl hexanoate, piperidines, 2,5 ?Er Jia Ji ?3 ?methyl, 1,5 ?heptadiene four kinds of novel substances.Wherein ethyl butyrate and ethyl hexanoate account for the massfraction of total material is respectively 1.81% and 0.25%.
Oxygenates level (area normalization method) 4.06% in sweet orange oil former state, limonene 91.62%.Product 6 oxygenates level 3.16%, limonene 93.2%, and wherein ethyl butyrate and ethyl hexanoate account for the massfraction of total material is respectively 1.81% and 0.25%.Ethyl hexanoate and ethyl butyrate account for 65.19% of the total oxygenatedchemicals of product 6.Obviously can change the odour characteristics of sweet orange oil, the odour characteristics of ethyl hexanoate and ethyl butyrate also can significantly embody simultaneously.Conform to the evaluation of the fragrant teacher of product.
Embodiment 6
Orange essential oil (Zhen Yun spices company limited provides by Guangzhou) 20mL is measured in 50mL tool plug port grinding bottle with graduated cylinder, in tool plug port grinding bottle, adding lipase PCALB again, (prepared by Chinese invention patent ZL200910039860.5 embodiment 4 method, enzyme is lived as 2000U/g) 0.2g, add the butyric acid of 420 μ l again, the acetic acid of 52 μ l, the caproic acid of 52 μ l, the leaf-alcohol of 50 μ l, the dehydrated alcohol of 450 μ l, then tool plug port grinding bottle is placed in constant-temperature table, at 55 DEG C, under 250r/min condition, carry out enzymatic reaction, 12h termination reaction.Filter and remove lipase, the orange essential oil room temperature after filtration is placed and within 3 days, can be obtained stable pure natural flavouring orange essential oil, called after product 8.
After product 8 and orange essential oil former state room temperature are placed 3 days, sample presentation please the fragrant slip-stick artist of product be evaluated.
Product fragrant teacher evaluate: the fragrance of product 8 has obvious change compared with the fragrance of former state sweet orange oil, and in product 8, the fragrance of ethyl butyrate, ethyl hexanoate all can obviously embody.
Sample pretreating method and GC ?MS detection method are as introduced in embodiment.GC ?MS detect find ethyl butyrate, β ?firpene, ethyl hexanoate, 1 ?Jia Ji ?4 ?(1 ?ethyl) ?tetrahydrobenzene, anti-Shi ?limonene oxide compound, Ding Suan ?3 ?hexene ester six kinds of novel substances.The mass ratio that wherein oxygenatedchemicals accounts for total material has risen to 2.6% from 0.47% of former state.Wherein ethyl butyrate and ethyl hexanoate account for respectively the massfraction (area normalization method) of total material be 1.63% and 0.3%, Ding Suan ?3 ?hexene ester account for 0.14% of total material mass mark.
Oxygenatedchemicals is the main aroma component in orange essential oil, by GC ?the data of MS can draw, the oxygenatedchemicals massfraction in orange essential oil former state is 0.47%.In product 8, ethyl butyrate and ethyl hexanoate account for the massfraction of total material is respectively 1.63% and 0.3%.Therefore, ethyl butyrate and ethyl hexanoate significantly change the odour characteristics of orange essential oil.The fragrance of ethyl butyrate and ethyl hexanoate also can embody simultaneously.Consistent with the evaluation of the fragrant slip-stick artist of product.
Application number is 201110461556.7 Chinese invention patent applications open (publication number CN102559386A).Disclose a kind of citrus essential oil and refine concentrated preparation method, the high efficiency separation of terpene compound and terpenes oxide compound in citrus essential oil is achieved by molecular distillation technique, make to heat up in a steamer remaining oxide content can be increased to original 5 ?20 times, the fragrance having heightened essential oil is worth.The method needs to use molecular distillation equipment, and prepares flux finite, is unfavorable for that heavy industrialization is applied and cost is more expensive.Embodiment 6 makes the concentration of oxygenatedchemicals in tangerine oil bring up to 1.97% by 0.47%, low price by adding simple acid alcohol under the effect of lipase, and processing flux is large, and the cycle is short, has significant advantage.
Claims (7)
1. an enzymatic method preparation method for natural flavouring tangerine oil, is characterized in that: added by lipase in tangerine oil, 35 ~ 60 DEG C, under 100 ~ 300RPM condition, reacts 4 ~ 24 hours, solids removed by filtration lipase, obtains natural flavouring tangerine oil; Every milliliter of tangerine oil adds the amount 0.01 ~ 0.05 gram of lipase.
2. the enzymatic method preparation method of natural flavouring tangerine oil according to claim 1, is characterized in that: described lipase is added in tangerine oil also to comprise add alcohol; The amount of the alcohol added is 0.5 ~ 5.0% of tangerine oil volume.
3. the enzymatic method preparation method of natural flavouring tangerine oil according to claim 2, is characterized in that: added by lipase in tangerine oil and alcohols also to comprise and add acid; The acid added and the mol ratio of alcohol are 1:1 ~ 1:5.
4. the enzymatic method preparation method of natural flavouring tangerine oil according to claim 1, is characterized in that: described lipase is the lipase with esterification function; In reaction system, the enzyme work of every gram of lipase is higher than 400U.
5. the enzymatic method preparation method of the natural flavouring tangerine oil according to Claims 2 or 3, is characterized in that: described alcohol be fermentable produce ethanol, lemongrass or Geraniol.
6. the enzymatic method preparation method of natural flavouring tangerine oil according to claim 3, is characterized in that: described acid is the natural acids of microorganism by fermentative production.
7. the enzymatic method preparation method of natural flavouring tangerine oil according to claim 6, is characterized in that: described natural acids is one or more in caproic acid, acetic acid, butyric acid and capric acid.
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| CN106389175A (en) * | 2016-09-07 | 2017-02-15 | 广州市澳键丰泽生物科技股份有限公司 | Nourishing and moisturizing lotion containing rose essential oil |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106389175A (en) * | 2016-09-07 | 2017-02-15 | 广州市澳键丰泽生物科技股份有限公司 | Nourishing and moisturizing lotion containing rose essential oil |
| CN106389175B (en) * | 2016-09-07 | 2019-06-07 | 广州市澳键丰泽生物科技股份有限公司 | A kind of nourishing and moisturizing lotion containing Rosa Damascana |
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