CN103087822B - Preparation method of glutinous essence - Google Patents

Abstract

The invention discloses a preparation method of glutinous essence. The preparation method comprises the following steps of: by taking orange peel as a raw material, obtaining orange peel enzymatic hydrolysate by utilizing the combined action of pectinase and cellulose and combining a hot water extraction process, and preparing natural glutinous essence through a Maillard reaction by taking the orange peel enzymatic hydrolysate as a reaction substrate. According to the preparation method of the glutinous essence, disclosed by the invention, by utilizing the high efficiency and the specificity of a biological enzyme method, macromolecules in the organic peel are subjected to enzymolysis to obtain the substrate required by the Maillard reaction, the conditions of the enzymolysis is gentle and is environment-friendly, the quality of the prepared glutinous essence is good, and the prepared glutinous essence has the advantages of low requirements in processes and devices, low energy consumption and the like; and the disadvantages of complex treatment after a chemical method, deep color of the obtained product, poor quality and the like are avoided.

Description

A kind of preparation method of glutinous taste essence

(1) technical field

The present invention relates to a kind ofly take orange peel and prepare the novel method of the glutinous taste essence of natural thermal response as raw material.

(2) background technology

Essence is by artificial allotment or by the mixture that contains multiple fragrant composition of the method manufactures such as fermentation, enzymolysis, thermal response.Essence and people's life is closely bound up, and people's life has be unable to do without the existence of essence day by day, is accompanied by the development of social materials culture, and people also constantly increase the kind of essence and demand, also day by day harsh to the requirement of the quality of essence.

The production method of essence has a lot, comprises the methods such as blending, fermentation, thermal response, enzymolysis.Thermal-reactive essence is a kind of novel food flavour, and just rise recent years, and it is heated under given conditions and produced through the reaction of series of complex by two or more " precursor substance ".Thermal response is again nonenzymatic browning reaction or Maillard reaction.International flavouring agent industrial organization (IOFI) is defined as follows hot reaction essence: hot reaction essence is product prepared by a kind of heating raw materials that has food raw material and allow to add in food or reaction essence.

When french chemist Luois Malilard in 1912 finds that glycine heats together with glucose, form the melanoidin of browning reaction.Through further studying, found that this type of reaction on the formation impact of the color of food and fragrance greatly afterwards.The kind of thermal response is varied, complicated mechanism, but ultimate principle has square to follow, and reaction base type is reducing sugar and amino acid whose reacting by heating.Studies show that, reacting between amino acid and reducing sugar is the main source that forms various heated foods fragrance.But in actual application, raw material is changeable, except amino acid and reducing sugar, other can participate in reacting and affect the formation of local flavor as VITAMIN, protein, fat etc.

Oranges and tangerines are the large fruit of the first in the world, and 2003 gross annual output amounts are 1.02 hundred million tons, account for 21.59% of world's fruit ultimate production.In recent years, China's orange yield is surged, and plants first of the area Yi Ju world, develops into 1,300,000 hectares, and annual production reaches 0.12 hundred million ton, surpasses the U.S. and occupies second.Wherein, wide skin tangerine accounts for more than 55%, and sweet orange accounts for 30%, and shaddock accounts for 10%, and other are 5% years old.Oranges and tangerines are first fruit in Zhejiang Province, and the whole province's cultivated area reaches 185.8 ten thousand mu, 163.8 ten thousand tons of ultimate productions at present.Since nineteen ninety-four, continuous 7 years positions of oranges and tangerines ultimate production are the first in the nation.Along with the development of citrus processing industry, left a large amount of byproducts, only the canned mandarin orange enterprise in Zhejiang Province, just approximately consumes 280,000 tons of satsuma oranges every year, and discarded orange peel reaches 5.6 ten thousand tons.According to research reports, in these discarded orange peels, it is heavy by 10% that exocarp accounts for fruit, is rich in volatile oil and pigment; Mesocarp accounts for the heavy 10-30% of fruit, and Mierocrystalline cellulose, pectin account for respectively 40% and 20% of whole mesocarp (dry weight); It is heavy by 10% that endocarp accounts for fruit, and in dry-matter, approximately containing half fiber of 44% sugar and 33% and Mierocrystalline cellulose, 20% pectin and xylogen, pentose glue class, other compositions also have glycoside, as hesperidine, vitamin P and obacalactone etc.

Contriver found through experiments, and the enzymolysis solution of orange peel contains the necessary amino acid of Maillard reaction and reducing sugar, has sprouted thus and has utilized tangerine peel to produce the research of Mei Lade hot reaction essence.

The food that traditional method is made is due to reasons such as making method are meticulous, heat-up time is long, its fragrance is generally all very abundant full, but adopt state-of-the-art facility food extensive, that produce fast, due to the reason such as process period on streamline is short, there is certain gap in its fragrance food general and that traditional method is made, this just needs the material of extra interpolation complementary flavor, Here it is food flavor(ing).And hot reaction essence as a kind of novel food flavour have give off a strong fragrance, the feature that mellow and full, mouthfeel is mellow, true to nature.Meanwhile, the essence that utilizes Maillard reaction to generate thinks to belong to natural essence category in the world, by FDA (Food and Drug Adminstration) (FDA), is assert it is to It is generally accepted safe product (GRAS).Maillard reaction essence also has many important functions, as reaction product all has good oxidation-resistance, can prevent fats oxidn, and bacteria growing inhibiting, can extend the goods quality guaranteed period effectively; On the impact of the absorption of mineral substance and excretion, there is the effect that is similar to foodstuff fibre; The restraining effect that nitrosamine is generated; Cancellation effect to excess oxygen; To immune physiological action and antimutagenic effect etc.The local flavor material that the Maillard of take reaction essence is main body is to people with back to nature circle, and the sensation of nutrition, safety, will become the leading product of Condiment Market from now on.

At present, very active to the research of Maillard reaction in the world, people utilize advanced science and technology and device separates and identify many Maillard reaction fragrance matters, and successfully synthesize on this basis and allocated beef flavour, chicken essence, pork essence etc. and take the seasonings that maillard reaction product (MRPs) is perfume base.From the patent documentation of delivering at present, American and Britain, De San state are mainly with at pure amino acid and sugar being synthetic MRPs flavorous condiment in the simulated system of main body, after therefrom understanding certain precursor heating, generate which fragrant composition and their generation approach and mechanism, review in this way the source of various fragrant compositions.Domestic a large amount of essence corporation and scientific research institution are mainly devoted to the research and development application of thermal response Meat flavor aroma.As Beijing Technology and Business University carries out the research of sulfur-bearing perfume material, Tsing-Hua University, Southern Yangtze University, Nankai University have carried out the research of heterocycle meat perfume material, Shanghai Brew Science Inst., the prosperous Food Co., Ltd in Chinese-foreign joint Shanghai, adopt yeast extract, application Maillard reaction novel process, new industrial research go out novel beef-meat paste seasonings etc.

Because the flavor compound that Maillard reaction produces is very complicated, adopt GC/MS to analyze more numerous and diverse to its aroma component, Electronic Nose is as the instrument of a kind of analysis, identification and detection of complex smell and most of volatile components, can give the Global Information of volatile component in sample, also claiming " fingerprint " data, is the ideal tools of the aroma substance of analysis ingredient complexity.Electronic Nose also claims Artificial Olfactory, is the olfactory function of the biological nose of simulation, thus a kind of electronic system that replaces human nose to detect.1993, the Gardner of Britain Warwick university, the Bart let of Southampton university have provided as given a definition Electronic Nose: Electronic Nose be a kind of by have part optionally chemical sensor array and suitable pattern recognition system form, can identify the instrument of simple or complicated smell.Through development for many years, Electronic Nose is more and more extensive in Application Areas, mainly concentrate on: the many-sides such as food, environment, agriculture production, medical treatment detection are especially remarkable at aspect effects such as drinks, meat, tealeaves, fruit maturation and storage period, essence identifications.

Electronic Nose is as new direction and the new technology of Food Quality and quality assessment, and oneself has its theoretical basis and application background.Electronic Nose has a wide range of applications in fields such as agricultural-food, Safety of Food Quality, foods supervisions, as: the discriminating of meat; The quality discrimination of wine and the differentiation of kind; The discriminating in the large feverfew place of production ^]; The differentiation of beverage classification; Pass judgment on cheese, Quality of Dairy Products; The control of wheat quality; Fruit and coffee aroma quality and maturity are judged; The food such as fish, meat freshness and quality judgement; The kind of Chinese medicinal materials, the place of production are differentiated; Detection of essence and flavoring agent etc.The characteristic such as kind, classification, quality that detects food by Electronic Nose has plurality of advantages: the state of testing sample is not had to special requirement, in most situation, the mensuration of sample is not lost to its this originality, do not destroy sample, what obtain is the Global Information of sample volatile flavor; Detection time is short, convenient and swift; The cost detecting is low, and testing sample is without the complicated loaded down with trivial details preprocessing process of process; Instrument is more general, can measure online and in real time, is easy to promote.

The research of current hot reaction essence is in the world very popular, and international Shi great essence corporation is if the companies such as IFF, Qi Huadun, Fen Meiyi are in the fund input aspect research and development.Technological development concentrates on the aspects such as synthetic technology, catalysis technique, analytical technology, biotechnology, novel separation and processing technology, essence novel process, novel form technology.The research integral body that contrasts domestic hot reaction essence is weaker, take meat essence as main.Can predict, strengthening from now on practical oranges and tangerines, to adopt the deep process technology research of rear high technology content be an inexorable trend, from Production trend and the utilization of resources, have more development potentiality and production development space, must promote China's oranges and tangerines to adopt rear industry fast development.

(3) summary of the invention

The object of the invention is to seek take orange peel as raw material, utilizes the acting in conjunction of polygalacturonase and cellulase and obtains orange peel enzymolysis solution in conjunction with hot water extracting technology, and the orange peel enzymolysis solution of further take reacts the method for preparing natural essence as reaction substrate by Maillard.

The technical solution used in the present invention is:

A kind of preparation method of glutinous taste essence, described method comprises the following steps: (1) gets dry orange peel powder, by the mass ratio of orange peel powder, water, be preferred 1:60 ~ 70 of 1:40 ~ 100() add water and be mixed to get mixed solution, under polygalacturonase and cellulase effect in 35 ~ 50 ℃ (preferably 45 ~ 50 ℃), pH 3.5 ~ 6.0(preferably 4.5 ~ 5.5) the preferred 100 ~ 150min of enzymolysis 90 ~ 180min(), then be warming up to 80 ~ 95 ℃ and extract preferably 100 ~ 120min of 60 ~ 150min(), centrifugal rear filtration, obtains filtrate and filter cake; The quality consumption of described polygalacturonase is the 0.01-0.04%(preferably 0.02 ~ 0.03% of mixed solution quality); The quality consumption of described cellulase is the 0.05-0.2%(preferably 0.1 ~ 0.15% of mixed solution quality);

(2) get filtrate and be concentrated into water content 80 ~ 98wt%, obtain concentrated solution;

(3) in step (2) gained concentrated solution, add L-Aspartic acid, polyvalent alcohol, described polyvalent alcohol is glycerine or propylene glycol, be preferably glycerine, after fully stirring, adjust pH is 5.0 ~ 8.0(preferably 7.0 ~ 7.5), then Maillard reaction is carried out in heating, at 110 ~ 150 ℃ of (preferably 130 ~ 140 ℃) temperature, react preferably 3 ~ 4h of 2 ~ 5h(), make described glutinous taste essence; The consumption of described L-Aspartic acid is counted 1/8 ~ 1/4 kg/L with the volume of concentrated solution, and the consumption of described polyvalent alcohol is counted 1/2 ~ 2/1 kg/L with the volume of concentrated solution.

Described step (2) can operate by the following method: get the filter cake that step (1) obtains, according to the extracting method of step (1), repeat to extract 1 ~ 3 time, merge all filtrate, be concentrated into water content 80 ~ 98wt%, obtain concentrated solution.

The enzyme work of polygalacturonase of the present invention is generally 30000u/g.The enzyme work of described cellulase is generally 40000u/g.

Concentrating normally at 50 ~ 70 ℃ of vacuum concentration in described step (2).

In step of the present invention (3), in gained concentrated solution, add L-Aspartic acid, polyvalent alcohol, the consumption of described L-Aspartic acid is counted 1/8 ~ 1/4 kg/L with the volume of concentrated solution, preferably 1/6 ~ 1/5 kg/L; The consumption of the polyvalent alcohol of described C3 is counted 1/2 ~ 2/1 kg/L with the volume of concentrated solution, preferably 1/1 ~ 2/1 kg/L.In concentrated solution, add after L-Aspartic acid, polyvalent alcohol, now the water content of reaction solution is 30 ~ 60wt% conventionally, and the water content of preferred reaction liquid is 30 ~ 50%, and most preferably water content is 40%.Can be by adding the consumption of L-Aspartic acid and polyvalent alcohol to adjust the water content in reaction solution.Water content of the present invention refers to: in the solution that the solute by water-soluble and aqueous solvent form, the quality percentage composition that aqueous solvent is shared, can measure according to standard GB 5009.3-2010 conventionally.

Dry orange peel powder of the present invention is by the coarse reduction of dry orange peel machinery, crosses 60 ~ 100 mesh sieves, obtains described dry orange peel powder.

In described step (3), the temperature of reaction is preferably 130 ~ 140 ℃, and the reaction times is preferably 3 ~ 4h, most preferably at 130 ℃, reacts 4 hours.

In described step (3), after fully stirring, adjust pH is 5.0 ~ 8.0, and preferably adjust pH is 7.0 ~ 7.5.In concentrated solution, add after L-Aspartic acid, polyvalent alcohol, not before adjust pH, the pH value of described reaction solution self is about 5.5 ~ 6.0, all can react pH value 5.0 ~ 8.0 is interior, can add adjusting PH with base value, do not regulate pH value also can react, but the present invention preferably add alkali (the NaOH aqueous solution of common available 0.2mol/L or the NaHCO of 0.2mol/L ₃the aqueous solution) being adjusted to pH value is 7.0 ~ 7.5 to react.

In described step (1), temperature of reaction during enzymolysis is preferably 45 ~ 50 ℃, and the reaction times is preferably 100 ~ 150min.

Comparatively preferred, recommend the method for the invention to carry out according to the following steps: (1) gets dry orange peel powder, by the mass ratio of orange peel powder, water, be that 1:60 ~ 70 add water and are mixed to get mixed solution, under polygalacturonase and cellulase effect in 45 ~ 50 ℃, pH 4.5 ~ 5.5 enzymolysis 100 ~ 150min, then be warming up to 80 ~ 95 ℃ and extract 100 ~ 120min, centrifugal rear filtration, obtains filtrate and filter cake; The quality consumption of described polygalacturonase is 0.02 ~ 0.03% of mixed solution quality; The quality consumption of described cellulase is 0.1 ~ 0.15% of mixed solution quality;

(2) get the filter cake that step (1) obtains, according to the extracting method of step (1), repeat to extract 1 ~ 3 time, merge all filtrate, 50 ~ 70 ℃ of vacuum concentration, to water content 80 ~ 98wt%, obtain concentrated solution;

(3) in step (2) gained concentrated solution, add L-Aspartic acid, polyvalent alcohol, described polyvalent alcohol is glycerine or propylene glycol, and after fully stirring, adjust pH is 7.0 ~ 7.5, and then Maillard reaction is carried out in heating, at 130 ~ 140 ℃ of temperature, react 3 ~ 4h, make described glutinous taste essence; The consumption of described L-Aspartic acid is counted 1/6 ~ 1/5 kg/L with the volume of concentrated solution, and the consumption of described polyvalent alcohol is counted 1/1 ~ 2/1 kg/L with the volume of concentrated solution.

The present invention be take orange peel as raw material, adopts enzymolysis process to obtain enzymolysis solution, by Maillard, is reacted and is obtained natural glutinous Flavor essence.The main points of invention are take that orange peel is as raw material, adopt enzymolysis process, react the natural flavour mountaineous essence obtaining by Maillard, give off a strong fragrance, round and smooth, true to nature, safety.

Beneficial effect of the present invention is mainly reflected in:

1. the present invention's thermal response material used is orange peel, adopts orange peel class material as the rarely seen report of raw material of hot reaction essence, and orange peel raw material is the byproduct of citrus processing, and the cost that is easy to get is low, safety non-toxic.

2. the natural flavour mountaineous essence that Maillard reaction of the present invention obtains, when high temperature, should not lose, be easy to other batchings concerted reaction occurs, make main aroma and other set off the more perfect coordination that fragrance embodies by contrast, the stereoscopic sensation that increases local flavor, gives back to nature circle, nutrition, the sensation of safety, has the incomparable effect of blending technology.

3. the present invention utilizes high efficiency and the specificity of biological enzyme, macromole in orange peel is carried out to enzymolysis acquisition Maillard and react required substrate, enzyme action condition is gentle, environmentally friendly, the good product quality obtaining, and to have the requirement of technique, equipment be not very high, low power consumption and other advantages.Avoided adopting chemistry (acid or alkali process hydrolysis) method aftertreatment complicated, the product colour of acquisition is dark, the bad deficiency that waits of quality.

(4) accompanying drawing explanation

The amino acid typical curve that Fig. 1 embodiment 1 step (4) obtains

The reducing sugar typical curve that Fig. 2 embodiment 1 step (5) obtains

The time dependent response curve of specific conductivity ratio of 6 sensors of Fig. 3 Electronic Nose.

The radar map that the essence that 9 kinds of orthogonal experiments of Fig. 4 make obtains through detection by electronic nose, respectively corresponding diagram 4-1 ~ 4-9

The essence that 9 kinds of orthogonal experiments of Fig. 5 make analyzes through the data of detection by electronic nose the PCA figure obtaining through PCA

(5) embodiment

Below in conjunction with specific embodiment, the present invention is described further, but protection scope of the present invention is not limited in this:

Embodiment 1

(1) preparation of raw material: clean Zhejiang Province and produce dry orange peel, remove impurity wherein, after pulverizing, cross 60 ~ 100 mesh sieves, obtain orange peel dry powder stand-by;

(2) reagent: 95% ethanol, glycerol, Xylene Brilliant Cyanine G reagent, DNS reagent; Glucose, bovine serum albumin.

(3) instrument: HMB-701C pulverizer, H1650 supercentrifuge, DHG-9240A electric drying oven with forced convection, the horizontal two storied gate refrigerating of BC/BD-199DSA Haier conversion cabinet, DK-8D electric heating constant temperature tank (temperature fluctuation: ± 0.5 ℃), RE-52A rotatory evaporator, and AL-104 electronic balance (scale division value: 0.0001g), T6 new millennium ultraviolet-visible pectrophotometer, HH-2 digital display thermostat water bath, LXJ-II centrifugal precipitation mechanism, vortex oscillation device, microwave oven etc.

(4) Xylene Brilliant Cyanine G method is surveyed amino acid

Xylene Brilliant Cyanine G reagent: Xylene Brilliant Cyanine G G-250 100mg is dissolved in 50ml 95% ethanol, adds 100ml 85% H ₃pO ₄, with distilled water diluting to 1000ml, filter paper filtering.In final reagent, contain 0.01%(W/V) Xylene Brilliant Cyanine G G-250,4.7%(W/V) ethanol, 8.5%(W/V) H ₃pO ₄.

Standard protein solution: pure bovine serum haemproteins, through micro-Kjeldahl, measure protein nitrogen content in advance, according to its purity, with 0.15mol/LNaCl, be mixed with 100ug/ml protein solution.

The making of table 1 amino acid typical curve

With A _595nmfor ordinate zou, standard protein content is X-coordinate (six points are 10ug, 20 ug, 30 ug, 40 ug, 50 ug, 60 ug), drawing standard curve in coordinate axis, and gained amino acid typical curve is shown in accompanying drawing 1.

The concentrated solution sample of getting in 0.5mL step (7) adds 0.15mol/L Nacl 0.5mL, then adds 5mL Xylene Brilliant Cyanine G reagent to shake up, and in 595nm place colorimetric, records experimental data together with above-mentioned typical curve.According to typical curve, can obtain aminoacids content in enzymolysis concentrated solution at 0.99mg/ml.

(5) DNS method is surveyed reducing sugar

Reagent: 3,5-edlefsen's reagent (claiming again DNS reagent); 0.1% glucose standardized solution: accurately take the glucose that 100 milligram analysises are pure (being dried to constant weight at 105 ℃ in advance), be settled to 100mL after dissolving with a small amount of distilled water, Refrigerator store is standby.

The making of table 2 reducing sugar typical curve

Take glucose concn as X-coordinate, optical density(OD) OD. ₅₀₀value is drawn out typical curve for ordinate zou, and the reducing sugar typical curve obtaining is shown in accompanying drawing 2.

In having scale 10mL colorimetric cylinder, add the concentrated solution sample 0.4mL (sample suitably dilution makes glucose concn within the scope of 0.05-1.0mg) in step (7), then add 3,5-edlefsen's reagent 1.2mL, mix, boiling water bath heating 5 minutes, cooling rapidly, adding distil water is to 10mL scale, shake up, the distilled water of usining replaces after sample simultaneous reactions as blank, photometry density on colorimeter, wavelength 540nm, light path 0.5cm.The content that can draw reducing sugar in enzymolysis concentrated solution according to typical curve is at 15.16mg/mL.That is to say that the content ratio of amino acid and reducing sugar in enzymolysis concentrated solution is probably in 1:15 left and right.

(6) processing of raw material: get orange peel dried powder 100g, adding quality is the deionized water of orange peel dry powder 60 times (6000g), mix and obtain mixed solution, add mixed solution quality 0.02% polygalacturonase (enzyme live for 30000u/g) and mixed solution quality 0.1% cellulase (enzyme is lived as 40000u/g), enzymolysis 150min under 45 ℃, the condition of pH5.0; Temperature is brought up to 90 ℃ again and extracted 120min, centrifugal, filtration, obtains filtrate and filter cake, gets filtrate and is concentrated into water content 92wt%, obtains concentrated solution 3.28L.

(7) Maillard reaction: will add the L-Aspartic acid of 0.55kg (1/6 kg/L) in concentrated solution, the add-on of glycerine adds by the requirement of water content in single factor below, stirs 120min, then use the NaHCO of 0.2mol/L in agitator ₃it is 7.0 that the aqueous solution is adjusted pH, puts into oil bath pan and heats.First adopt experiment of single factor, take local flavor as index, research water content, temperature of reaction, the impact of the factors such as reaction times on essence local flavor, according to the many orthogonal tests of experiment of single factor consequence devised.

Table 3 bath oiling single factor experiment table

(8) subjective appreciation method: adopt acceptable check, selected 8 subjective appreciation persons that see service sort by characteristic intensity and the hedonic scale of appointment to sample, and assessment officer is strong and weak with regard to glutinous taste to reacted local flavor material, glutinous taste soften and be charred strong and weak these three indexs of peculiar smell and mark respectively.With system scoring in 9 minutes, not liking was very much 1 minute, and not liking is 2 minutes very much, and not liking is 3 minutes, and not liking is 4 minutes, is generally 5 minutes, and slightly liking is 6 minutes, and liking is 7 minutes, and being delithted with is 8 minutes, and enjoying a lot is 9 minutes.Mark higher, show that the glutinous taste of sample is stronger, soften is higher, it is more weak to be charred easy taste smell.

Through subjective appreciation, 110 ~ 130 ℃ of temperature of reaction, in 2 ~ 4 hours reaction times, under the condition that water content is 30 ~ 50%, scoring is higher than under other single factor conditions, and selected above-mentioned condition is carried out following orthogonal experiment.

(9) orthogonal experiment and detection by electronic nose

According to single factor experiment repeatedly, design three level three factor orthogonal test conditions are as table 4.

Table 4 orthogonal test level of factor table

According to orthogonal test, prepare hot reaction essence, according to step (8), carry out subjective appreciation, fragrance comprehensive grading is as table 5.

Table 5 orthogonal experiments

Experiment number	A	B	C	Average score
					1	1	1	1	6.2
2	1	2	2	8.7
					3	1	3	3	8.4
4	2	1	2	6.7
					5	2	2	3	7.2
6	2	3	1	8.3
					7	3	1	3	6.9
8	3	2	1	7.7
					9	3	3	2	9.2
K 1	7.77	6.60	7.40	?
					K 2	7.40	7.87	8.30	?
K 3	7.93	8.63	7.50	?
					R	0.16	2.03	0.90	?

By orthogonal experiments, can be drawn, the reaction times has the greatest impact to the local flavor of hot reaction essence, and reaction temperatures affect is minimum.The top condition of preparing hot reaction essence is 130 ℃ of temperature of reaction, reaction times 4h, and water content is 40%.

Detection by electronic nose: instrument: α-Genemi type Electronic Nose France Alpha. MOS company produces.

Process approach: get essence sample after bath oiling orthogonal optimization after sealing for some time, its head space gas (sample gas) is injected in Electronic Nose through syringe sampling, in this Electronic Nose, be equipped with 6 sensors, be respectively PA/2, P30/1, P30/2, LY2/AA, LY2/gCT and T70/2, sensor is because having adsorbed a certain amount of volatile matter, specific conductivity changes, this signal is obtained and is stored in computer by data collecting system, to the data analysis obtaining, determine the taste compound of essence fragrance main body.

Fig. 3 is the time dependent response curve of specific conductivity ratio of 6 sensors of Electronic Nose.In this figure, every curve represents a sensor, and the point on curve represents when the fragrance ingredient of spices passes through sensor passage, relative resistance rate (G/G ₀) situation over time.As can be seen from the figure the response value of Electronic Nose sensor tended towards stability after 45 seconds, therefore 45 seconds later response values of collected specimens are analyzed.

The hot reaction essence that 9 kinds of orthogonal experiments make is through detection by electronic nose, and the radar map of the essence obtaining is respective figure 4-1 ~ 4-9 respectively:

The radar map of the essence being obtained by nine tests can be found out, the radar graphic of nine kinds of essence is not identical, and 5 in Electronic Nose in 6 sensors have strong response to essence sample, but the degree of each sample response exists obvious difference, in conjunction with the result to sample fragrance comprehensive grading, can find out to the highest No. 9 essence response of scoring the highest be P30/2 sensor.

Nine groups of essence prepared by PCA methods analyst differential responses condition, its PCA schemes as Fig. 5:

Principle component analysis (Principle Component Analysis, PCA) be a kind of multivariate statistical method, that the many indication informations of the sensor of extraction are carried out to data-switching and dimensionality reduction, and the proper vector after dimensionality reduction is carried out to linear classification, finally on PCA analysis chart, show main graphics.Horizontal (PC1), vertical (PC2) coordinate are illustrated respectively in the first principal component that obtains in PCA conversion and the contribution rate of Second principal component.Fig. 5 can find out, the contribution rate of first principal component is 88.039%, and the contribution rate of Second principal component, is 10.651%.The principal constituent that contribution rate is larger can reflect the information of former many indexs preferably.If two samples distance on X-coordinate is larger, illustrate that their difference is larger; And even two samples distance on ordinate zou is very large, but because the contribution rate of Second principal component, is very little, so the actual variance of two sample rooms can be not clearly yet.

More approaching from 9,2, No. 3 sample smells of PCA analysis chart.In conjunction with sensory test, the local flavor of 9,2, No. 3 samples and soften are best, and score is the highest, illustrates that the difference of these 3 samples is less, and flavour substances is close; And the sense organ score of 1,4, No. 5 sample is lower, be charred peculiar smell, in PCA analysis chart, the difference of these samples is very little.From PCA analysis chart, 9,2, No. 3 samples that 1,4, No. 5 sample that sense organ score is lower and sense organ score are higher have notable difference, illustrate that adopting PCA to analyze has certain difference degree to the sample of different process, can classify from large class.Adopt the PCA in Electronic Nose Technology to analyze, objective, smell analysis accurately and fast that flavour substances prepared by different process carries out, reproducible, consistent with Analyses Methods for Sensory Evaluation Results.That detection by electronic nose has is harmless, feature fast, and the rapid detection that test-results can be suitability for industrialized production flavor substances provides reference.

Embodiment 2

(1) preparation of raw material: clean Zhejiang Province and produce dry orange peel, remove impurity wherein, after pulverizing, cross 60 ~ 100 mesh sieves, obtain orange peel dry powder stand-by;

(2) processing of raw material: get orange peel dried powder 100g, adding quality is the deionized water of orange peel dry powder 40 times (4000g), add 0.04% polygalacturonase (enzyme live for 30000u/g) and 0.2% cellulase (enzyme is lived as 40000u/g), enzymolysis 180min under 45 ℃, the condition of pH5.0; Extraction temperature is brought up to 95 ℃ again and extracted 60min, centrifugal, filtration, obtains filtrate and filter cake, gets filtrate and is concentrated into water content 89wt%, obtains concentrated solution 1.76L.

(3) glycerine Maillard reaction: will add L-Aspartic acid, the 1.76kg(1/1 kg/L of 0.29kg (1/6 kg/L) in concentrated solution), controls water content 44%, stirs 120min, then use the NaHCO of 0.2mol/L in agitator ₃it is 7.5 that the aqueous solution is adjusted pH, puts into oil bath pan and heats, and the optimum reaction condition of optimizing by embodiment 1 obtains glutinous taste essence.

(4) subjective appreciation method: press the methods of marking of embodiment 1 step (8), this embodiment is equally divided into 7.15 minutes.

Embodiment 3

(1) preparation of raw material: clean Zhejiang Province and produce dry orange peel, remove impurity wherein, after pulverizing, cross 60 ~ 100 mesh sieves, obtain orange peel dry powder stand-by;

(2) processing of raw material: get orange peel dried powder 20g, adding quality is the deionized water of orange peel dry powder 100 times (2000g), add 0.01% polygalacturonase (enzyme live for 30000u/g) and 0.05% cellulase (enzyme is lived as 40000u/g), enzymolysis 90min under 50 ℃, the condition of pH4.0; Extraction temperature is brought up to 85 ℃ again and extracted 150min, centrifugal, filtration, obtains filtrate and filter cake, gets filtrate and is concentrated into water content 95wt%, obtains concentrated solution 0.92L.

(3) glycerine Maillard reaction: will add L-Aspartic acid, the 1.84kg(2/1 kg/L of 0.12kg (1/8 kg/L) in concentrated solution), controls water content 32%, stirs 120min, then use the NaHCO of 0.2mol/L in agitator ₃it is 8.0 that the aqueous solution is adjusted pH, puts into oil bath pan and heats, and the optimum reaction condition of optimizing by embodiment 1 obtains glutinous taste essence.

(4) subjective appreciation method: press the methods of marking of embodiment 1 step (8), this embodiment is equally divided into 6.85 minutes.

Embodiment 4

(1) preparation of raw material: clean Zhejiang Province and produce dry orange peel, remove impurity wherein, after pulverizing, cross 60 ~ 100 mesh sieves, obtain orange peel dry powder stand-by;

(2) processing of raw material: get orange peel dried powder 50g, adding quality is the deionized water of orange peel dry powder 80 times (4000g), add 0.03% polygalacturonase (enzyme live for 30000u/g) and 0.15% cellulase (enzyme is lived as 40000u/g), enzymolysis 150min under 40 ℃, the condition of pH5.5; Extraction temperature is brought up to 80 ℃ again and extracted 150min, centrifugal, filtration, obtains filtrate and filter cake, gets filtrate and is concentrated into water content 80wt%, obtains concentrated solution 1.54L.

(3) glycerine Maillard reaction: will add L-Aspartic acid, the 0.77kg(1/2 kg/L of 0.38kg (1/4 kg/L) in concentrated solution), control water content 53%, in agitator, stir 120min, with the HCl aqueous solution of 0.2mol/L, adjusting pH is again 6.0, put into oil bath pan and heat, the optimum reaction condition of optimizing by embodiment 1 obtains glutinous taste essence.

(4) subjective appreciation method: press the methods of marking of embodiment 1 step (8), this embodiment is equally divided into 8.125 minutes.

Comparative example 1

(1) preparation of raw material: clean Zhejiang Province and produce dry orange peel, remove impurity wherein, after pulverizing, cross 60 ~ 100 mesh sieves, obtain orange peel dry powder stand-by;

(2) processing of raw material: get orange peel dried powder 50g, adding quality is the deionized water of orange peel dry powder 60 times (3000g) is to extract 150min under 80 ℃ of conditions extracting temperature, centrifugal, filtration, obtain filtrate and filter cake, get filtrate and be concentrated into water content 90wt%, obtain concentrated solution 1.22L.

(3) glycerine Maillard reaction: will add L-Aspartic acid, the 1.22kg(1/1 kg/L of 0.15kg (1/8 kg/L) in concentrated solution), control water content 45%, in agitator, stir 120min, with the HCl aqueous solution of 0.2mol/L, adjusting pH is again 6.0, put into oil bath pan and heat, the optimum reaction condition of optimizing by embodiment 1 obtains glutinous taste essence.

(4) subjective appreciation method: press the methods of marking of embodiment 1 step (8), being equally divided into of this embodiment is 3.75 minutes.

Comparative example 2

(1) preparation of raw material: clean Zhejiang Province and produce dry orange peel, remove impurity wherein, after pulverizing, cross 60 ~ 100 mesh sieves, obtain orange peel dry powder stand-by;

(2) processing of raw material: get orange peel dried powder 50g, adding quality is the deionized water of orange peel dry powder 60 times (3000g) is to extract 120min under 95 ℃ of conditions extracting temperature, centrifugal, filtration, obtain filtrate and filter cake, get filtrate and be concentrated into water content 85wt%, obtain concentrated solution 1.14L.

(3) glycerine Maillard reaction: will add L-Aspartic acid, the 1.22kg(1/2 kg/L of 0.28kg (1/4 kg/L) in concentrated solution), controls water content 56%, stirs 120min, then use the NaHCO of 0.2mol/L in agitator ₃it is 7.0 that the aqueous solution is adjusted pH, puts into oil bath pan and heats, and the optimum reaction condition of optimizing by embodiment 1 obtains glutinous taste essence.

(4) subjective appreciation method: press the methods of marking of embodiment 1 step (8), being equally divided into of this embodiment is 4.75 minutes.

Claims (8)

1. the preparation method of a glutinous taste essence, it is characterized in that described method comprises the following steps: (1) gets dry orange peel powder, by the mass ratio of orange peel powder, water, be that 1:40 ~ 100 add water and are mixed to get mixed solution, under polygalacturonase and cellulase effect in 35 ~ 50 ℃, pH 3.5 ~ 6.0 enzymolysis 90 ~ 180min, then be warming up to 80 ~ 95 ℃ and extract 60 ~ 150min, centrifugal rear filtration, obtains filtrate and filter cake; The quality consumption of described polygalacturonase is the 0.01-0.04% of mixed solution quality; The quality consumption of described cellulase is the 0.05-0.2% of mixed solution quality;

(2) get filtrate and be concentrated into water content 80 ~ 98wt%, obtain concentrated solution;

(3) in step (2) gained concentrated solution, add L-Aspartic acid, polyvalent alcohol, described polyvalent alcohol is glycerine or propylene glycol, and after fully stirring, adjust pH is 5.0 ~ 8.0, and then Maillard reaction is carried out in heating, at 110 ~ 150 ℃ of temperature, react 2 ~ 5h, make described glutinous taste essence; The consumption of described L-Aspartic acid is counted 1/8 ~ 1/4 kg/L with the volume of concentrated solution, and the consumption of described polyvalent alcohol is counted 1/2 ~ 2/1 kg/L with the volume of concentrated solution.

2. the method for claim 1, it is characterized in that described step (2) operates by the following method: get the filter cake that step (1) obtains, according to the extracting method of step (1), repeat to extract 1 ~ 3 time, merge all filtrate, be concentrated into water content 80 ~ 98wt%, obtain concentrated solution.

3. method as claimed in claim 1 or 2, is characterized in that described concentrating is at 50 ~ 70 ℃ of vacuum concentration.

4. method as claimed in claim 1 or 2, is characterized in that described dry orange peel powder is by the coarse reduction of dry orange peel machinery, crosses 60 ~ 100 mesh sieves, obtains described dry orange peel powder.

5. method as claimed in claim 1 or 2, is characterized in that, in described step (3), the temperature of reaction is 130 ~ 140 ℃, and the reaction times is 3 ~ 4h.

6. method as claimed in claim 1 or 2, is characterized in that in described step (3), and after fully stirring, adjust pH is 7.0 ~ 7.5.

7. method as claimed in claim 1 or 2, is characterized in that, in described step (1), temperature of reaction during enzymolysis is 45 ~ 50 ℃, and the reaction times is 100 ~ 150min.

8. method as claimed in claim 2, it is characterized in that said method comprising the steps of: (1) gets dry orange peel powder, by the mass ratio of orange peel powder, water, be that 1:60 ~ 70 add water and are mixed to get mixed solution, under polygalacturonase and cellulase effect in 45 ~ 50 ℃, pH 4.5 ~ 5.5 enzymolysis 100 ~ 150min, then be warming up to 80 ~ 95 ℃ and extract 100 ~ 120min, centrifugal rear filtration, obtains filtrate and filter cake; The quality consumption of described polygalacturonase is 0.02 ~ 0.03% of mixed solution quality; The quality consumption of described cellulase is 0.1 ~ 0.15% of mixed solution quality;

(2) get the filter cake that step (1) obtains, according to the extracting method of step (1), repeat to extract 1 ~ 3 time, merge all filtrate, 50 ~ 70 ℃ of vacuum concentration, to water content 80 ~ 98wt%, obtain concentrated solution;

(3) in step (2) gained concentrated solution, add L-Aspartic acid, polyvalent alcohol, described polyvalent alcohol is glycerine or propylene glycol, and after fully stirring, adjust pH is 7.0 ~ 7.5, and then Maillard reaction is carried out in heating, at 130 ~ 140 ℃ of temperature, react 3 ~ 4h, make described glutinous taste essence; The consumption of described L-Aspartic acid is counted 1/6 ~ 1/5 kg/L with the volume of concentrated solution, and the consumption of described polyvalent alcohol is counted 1/1 ~ 2/1 kg/L with the volume of concentrated solution.