CN104237403A - Method for distinguishing chicken base - Google Patents
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- CN104237403A CN104237403A CN201410444679.3A CN201410444679A CN104237403A CN 104237403 A CN104237403 A CN 104237403A CN 201410444679 A CN201410444679 A CN 201410444679A CN 104237403 A CN104237403 A CN 104237403A
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Abstract
The invention discloses a method for distinguishing chicken base. The method comprises the following steps: firstly preparing the chicken base by adopting chicken protein enzymatic hydrolysate through maillard reaction, acquiring and analyzing volatile flavor matters in the chicken base by utilizing a headspace gas chromatography-mass spectrometer, distinguishing the chicken base by virtue of PCA-HCA (main component-clustering analysis), and distinguishing the chicken base in a sense organ evaluation method. The method for distinguishing the chicken base is comprehensive, reasonable and capable of effectively distinguishing the chicken base.
Description
Technical field
The invention belongs to detection analysis field, particularly relate to a kind of method that chicken perfume base is distinguished.
Background technology
Be rich in free amino acid and peptide in chicken enzymolysis liquid, both participate in Maillard reaction is important Flavor Prccursors.In the present invention, the preparation of chicken perfume base is the flavor substance obtained by Maillard reaction and the thiamine degradation reaction of reducing sugar and amino acid and peptide.
Volatile ingredient in chicken is of a great variety, mainly comprises nitrogen-containing compound, sulfocompound, carbonyls.Wherein 2-furfuryl mercaptan, 2-methyl-3-sulfydryl furans, two (2-methyl-3-furyl) disulfide etc. are important chicken perfume compounds.Traditional meat products local flavor is probed into and is depended on two kinds of mode (1) sensory evaluation personnel to the subjective assessment of sample sensory attribute; (2) by means of gas chromatography-mass spectrometry analysis instrument, qualitative and quantitative analysis is carried out to aroma substance.On the one hand, by the impact of sensory evaluation personnel individual difference and the restriction of aroma substance threshold value height, evaluation result has uncertainty and instability.On the other hand, the qualitative and quantitative analysis of gas chromatograph-mass spectrometer (GCMS) to aroma substance local flavor makes analytic process numerous and diverse, increases workload, and have ignored the modified tone effect between the Flavor of perfume base and aroma substance to a certain extent.Principal component analysis (PCA) is by numerous index with certain correlativity, is reassembled into the dimension that one group of new overall target irrelevant mutually reduces data set, keeps data set to the maximum feature of variance contribution simultaneously.Principal component analysis (PCA) and cluster analysis are carried out to kind of the key odorant material of 34 in chicken perfume base, probes into the impact of chicken protein hydrolysate addition on chicken perfume base local flavor.Subjectivity and the uncertainty of naked eyes evaluation is compensate for by objective Mathematical Statistics Analysis, the dimensionality reduction effect of principal component analysis (PCA) simplifies analytic process, cluster analysis is then classified to sample by the Integral Differential opposite sex, mathematical statistics and sensory evaluation is incorporated into sector-style taste and probes into and make evaluation result comprehensively, rationally.
Summary of the invention
For above-mentioned technical matters of the prior art, the invention provides a kind of method that chicken perfume base is distinguished, described this method will solve headspace gas chromatography-GC-MS cannot carry out concentrated expression technical matters to the overall flavor characteristic of chicken perfume base, efficiently solve simultaneously sensory evaluation personnel individual difference and aroma substance threshold value height on local flavor analyze impact, reduce uncertainty and the instability of evaluation result, reduce the workload that local flavor is analyzed simultaneously.
A kind of method distinguished chicken perfume base of the present invention, comprises the steps:
(1), the step of chicken perfume base is prepared for one:
(2), one is carried out the step of headspace gas chromatography-mass spectrophotometry mensuration to the different chicken perfume base samples of step (1) gained:
, get chicken perfume base sample 8g respectively, sodium chloride 1g puts into 15mL or 20ml ml headspace bottle, 65 ~ 75 DEG C of water-baths balance 10min, in 65 ~ 75 DEG C of water-baths, SPME head space Static Adsorption 60min;
, by SPME extracting head, the gas chromatographic sample introduction mouth inserted in headspace gas chromatography-GC-MS is resolved, resolution temperature 250 DEG C, resolves time 5min, different chicken perfume base samples is carried out to the mensuration of volatile ingredient;
In described headspace gas chromatography-GC-MS, gas chromatography condition of work:
Mm × 0.25 μm, HP-INNOWAX(60 m × 0.25) chromatographic column; Heating schedule: initial temperature is set to 50 DEG C, keeps 2min, with the ramp to 230 DEG C of 4 DEG C/min, maintains 10min; Carrier gas He, flow velocity 1mL/min; Splitless injecting samples;
Mass spectrum condition of work: solvent delay 3min, ion source temperature 230 DEG C, EI ionization source, electron energy 70eV, sweep limit 30-450amu;
, qualitative and quantitative analysis is carried out to the volatile ingredient in chicken perfume base sample: the mass spectrometric data in the volatile ingredient mensuration process in above-mentioned different chicken perfume base sample mated with 3 standard spectrum storehouses MAINLIB, NISTDEMO, WILLEY in computer chemistry workstation, By consulting literatures retention index carries out qualitative analysis; Carry out quantitative test in conjunction with interior scalar quantity and peak area ratio to mate with 3 standard spectrum storehouses MAINLIB, NISTDEMO, WILLEY in chem workstation, By consulting literatures retention index carries out qualitative analysis;
(3), Dimension Reduction Analysis and cluster analysis is carried out by the different chicken perfume base volatile ingredient qualitative and quantitative analysis results of PCA-HCA to above-mentioned steps (2) gained, in conjunction with sense organ descriptive analysis, subjective fragrance description is carried out to chicken perfume base sample, Flavor analysis is carried out to chicken perfume base, thus chicken perfume base sample is distinguished.
Further, the step preparing chicken perfume base is as follows:
1) chicken breast meat is taken respectively, deionized water and compound protease, described chicken breast meat, the weight ratio of deionized water and compound protease is 1:3:0.003, and by chicken breast meat, deionized water and compound protease add in a reaction vessel, 45 ~ 55 DEG C of enzymolysis 2 ~ 4h, cooling obtains chicken enzymolysis liquid;
2), take the chicken enzymolysis liquid that step 1) obtains respectively, deionized water, glucose, wood sugar, cysteine salt, glycocoll, alanine, thiamine, salt and monosodium glutamate, described chicken enzymolysis liquid, deionized water, glucose, wood sugar, cysteine salt, glycocoll, alanine, thiamine, the weight ratio of salt and monosodium glutamate is 39:13:1:0.5:1:0.5:0.5:1:3:0.5, by chicken enzymolysis liquid, deionized water, glucose, wood sugar, cysteine salt, glycocoll, alanine, thiamine, salt and monosodium glutamate add in another one reaction vessel, under the condition of pH 7.5 ~ 9.0,105 ~ 110 DEG C of oil bath reaction 0.5 ~ 1.5h obtain chicken perfume base.
Further, aroma volatile in chicken perfume base is being carried out in the step of PCA-HCA analysis, utilize statistical software XLSTAT2010 to carry out PCA and HCA to the aroma substance of qualitative, quantitative in chicken perfume base to analyze, first centralization process and nondimensionalization process are carried out to data, after process, data point carries out PCA Dimension Reduction Analysis according to covariance arithmetic, obtain each data point and the sample distribution plan at first principal component and Second principal component, according to Euclidean distance method and sum of squares of deviations method (Ward's method), HCA cluster analysis is carried out to sample, obtain sample classification figure.
Further, described Volatile infochemicals comprises: 2-furfuryl mercaptan, 3-methylpyrrole, 2-acetyl pyrrole, 2-methyl-3-hydroxyl-pyrokomane, 2-methylfuran, 2-amyl furan, 2-methyl-3-sulfydryl furans, 2-acetyl furan, two (2-methyl-3-furyl) disulfide, 3-methylbutyraldehyd, hexanal, aldehyde C-9, 2-octenal, furfural, benzaldehyde, 2-methylthiophene, n-octyl alcohol, pyrazine, thiazole, 4-methylthiazol, 2-acetylthiazole, 4-methyl-5-hydroxy ethylthiazole, 2-methyltetrahydrofuran-3-ketone, methyln-hexyl ketone, 3-sulfydryl-2 pentanone, 2-HEPTANONE, Ergol, formic acid, acetic acid, caproic acid, sad, dodecoic acid, tetradecylic acid and hexadecylic acid.
The present invention is by the Volatile infochemicals in chicken perfume base sample through headspace gas chromatography-GC-MS qualitative, quantitative, and data, through centralization and nondimensionalization process, are then carried out PCA and analyzed and HCA analysis.PCA analyzes by covariance (Covariance(n)) each data point and chicken perfume base sample be projected in first principal component (X-axis) and Second principal component, (Y-axis) by algorithm.HCA analyzes and carries out cluster analysis by Euclidean distance method (Eudidean distance) and sum of squares of deviations method (Ward's method) to sample.Carry out sensory evaluation scores in conjunction with sense organ descriptive analysis to above-mentioned graded samples to distinguish sample.
The present invention is a kind of method utilizing headspace gas chromatography-GC-MS to distinguish chicken perfume base in conjunction with PCA-HCA and sensory evaluation, owing to adopting headspace gas chromatography-GC-MS in conjunction with PCA-HCA, while to the volatile ingredient qualitative and quantitative analysis in chicken perfume base sample, the overall local flavor difference of chicken perfume base is obtained by PCA reduction dimensional analysis and HCA cluster analysis, in conjunction with the subjective analysis of sensory evaluation personnel, differentiation result is tending towards comprehensively, rationally, science.
Accompanying drawing explanation
Fig. 1 is step (3) PCA data profile in embodiment 1, as can be seen from Figure 1 major component 1 contribution rate is 70.62%, major component 2 contribution rate is 20.72%, contribution rate of accumulative total is 91.34%, therefore gets major component 1 and major component 2 and represent the volatile flavor substance that headspace gas chromatography-GC-MS records.
Fig. 2 is step (3) PCA sample distribution figure in embodiment 1.
Fig. 3 is step (3) sample HCA(cluster analysis figure in embodiment 1), as can be seen from Figure 3 sample A and other samples are divided into two large classes, and sample B and sample C, D, E belong to two subclass, and in the second subclass, sample E distinguishes over again sample C and D.
Fig. 4 is step (3) sample HCA(cluster analysis figure in embodiment 1), C1 representative sample A in Fig. 4, C2 representative sample B, C3 representative sample C, D, E.
Embodiment
Also by reference to the accompanying drawings the present invention is set forth further below by specific embodiment, but do not limit the present invention.
Embodiment 1
The method utilizing headspace gas chromatography-GC-MS to distinguish chicken perfume base in conjunction with PCA-HCA and sensory evaluation, specifically comprises the following steps:
(1), chicken perfume base preparation of samples:
Get commercially available fresh chicken breast meat (1 parts by weight), deionized water 3(parts by weight), compound protease (0.3% parts by weight), under pH6.5 condition, 50 DEG C of water-baths, speed of agitator 800 revs/min, enzymolysis 3h, go out enzyme 10 minutes in 100 DEG C of water-baths, and cooling obtains chicken enzymolysis liquid; Chicken enzymolysis liquid (39 parts by weight), deionized water (13 parts by weight), glucose (1 parts by weight), wood sugar (0.5 parts by weight), cysteine salt (1 parts by weight), glycocoll (0.5 parts by weight), alanine (0.5 parts by weight), thiamine (1 parts by weight), salt (3 parts by weight) and monosodium glutamate (0.5 parts by weight) 108 DEG C of oil bath reaction 1h under the condition of pH8.0 obtain five kinds of chicken perfume base samples A, B, C, D and E;
(2), respectively carry out headspace gas chromatography-mass spectrophotometry mensuration to the chicken perfume base sample of step (1) gained, detailed process is as follows:
, get chicken perfume base sample 8g respectively, sodium chloride 1g puts into 15mL ml headspace bottle, 70 DEG C of water-baths balance 10min, in 70 DEG C of water-baths, SPME head space Static Adsorption 60min;
Described SPME extracting head is 75 μm of CAR/PDMS, Supelco companies;
, by SPME extracting head, the gas chromatographic sample introduction mouth inserted in headspace gas chromatography-GC-MS is resolved, resolution temperature 250 DEG C, resolves time 5min, different chicken perfume base samples is carried out to the mensuration of volatile ingredient;
In described headspace gas chromatography-GC-MS, gas chromatography condition of work:
Mm × 0.25 μm, HP-INNOWAX(60 m × 0.25) chromatographic column; Heating schedule: initial temperature is set to 50 DEG C and keeps 2min, with the ramp to 230 DEG C of 4 DEG C/min, maintains 10min; Carrier gas He, flow velocity 1mL/min; Splitless injecting samples;
Mass spectrum condition of work: solvent delay 3min, ion source temperature 230 DEG C, EI ionization source, electron energy 70eV, sweep limit 30-450amu;
, by the mass spectrometric data in the volatile ingredient mensuration process in above-mentioned different chicken perfume base sample and computing machine
3 standard spectrum storehouse MAINLIB, NISTDEMO, WILLEY couplings in chem workstation, By consulting literatures retention index carries out qualitative analysis; Internal standard method is adopted to carry out quantitative computing formula: Ni=fi ×
× Ws, in formula, fi correction factor is 1, Ai component peaks area to be measured, the peak area of As internal standard compound, the quality of Ws internal standard compound, Ni test substance quality;
The effective volatile ingredient analyzed in the present invention comprises: 1(2-furfuryl mercaptan), 2(3-methylpyrrole), 3(2-acetyl pyrrole), 4(2-methyl-3-hydroxyl-pyrokomane), 5(2-methylfuran), 6(2-pentyl furan), 7(2-methyl-3-sulfydryl furans), 8(2-acetyl furan), two (2-methyl-3-furyl) disulfide of 9(), 10(3-methylbutyraldehyd), 11(hexanal), 12(aldehyde C-9), 13(2-octenal), 14(furfural), 15(benzaldehyde), 16(2-methylthiophene), 17(n-octyl alcohol), 18(pyrazine), 19(thiazole), 20(4-methylthiazol), 21(2-acetylthiazole), 22(4-methyl-5-hydroxy ethylthiazole), 23(2-methyltetrahydrofuran-3-ketone), 24(2-octanone), 25(3-sulfydryl-2 pentanone), 26(2-heptanone), 27(Ergol), 28(formic acid), 29(acetic acid), 30(caproic acid), 31(is sad), 32(dodecoic acid), 33(tetradecylic acid) and 34(hexadecylic acid),
(3), to the aroma volatile in the chicken perfume base of qualitative, quantitative in step (2) carry out PCA-HCA analysis, concrete steps are as follows:
Utilize statistical software XLSTAT2010 to carry out PCA and HCA to 34 kinds of aroma substances of qualitative, quantitative in step (2) chicken perfume base to analyze, first centralization process and nondimensionalization process are carried out to data, after process, data point is according to covariance (Covariance(n)) algorithm carries out PCA Dimension Reduction Analysis, obtain each data point and the sample distribution plan (see Fig. 1 and Fig. 2) at first principal component and Second principal component, take first principal component as X-axis contribution rate be 70.62%, Second principal component, is Y-axis contribution rate is 20.72%; According to Euclidean distance method (Eudidean distance) and sum of squares of deviations method (Ward's method), HCA cluster analysis is carried out to sample, obtain sample classification figure (see Fig. 3 and Fig. 4 Suo Shi);
(4) sense organ descriptive analysis, is utilized to carry out sensory evaluation scores concrete steps to chicken perfume base sample prepared by step (1) as follows:
Select the age 25-45 one full year of life 6 male 4 female, 10 the sense organ appraise composition of personnel sense organ appraise groups being engaged in flavour of food products research work according to ISO 8586-1:1993 (E) standard to appraise staff training; Smell to hear and taste to chicken perfume base and obtain meat perfume, burnt odor, fresh perfume (or spice), persistence and peculiar smell 5 kinds of sensory attribute; Carry out aroma strength marking (0 represents extremely weak, and 9 represent extremely strong) according to 0-9 ten point system, obtain chicken perfume base sample marking result (see table 1);
Table 1 chicken perfume base sample sense organ descriptive analysis tables of data
Step (4) sense organ descriptive analysis tables of data in table 1, embodiment 1, the outstanding burnt odor local flavor of sample A entirety as can be seen from Table 1, the outstanding meat Flavor of sample B entirety, sample C, D, E be overall outstanding fresh Flavor and peculiar smell then, illustrates that in chicken perfume base preparation process, chicken enzymolysis liquid is remarkable to overall flavor effect.
Foregoing be only the present invention conceive under basic explanation, and according to any equivalent transformation that technical scheme of the present invention is done, all should scope be belonged to.
Claims (4)
1., to the method that chicken perfume base is distinguished, it is characterized in that comprising the steps:
(1), the step of chicken perfume base is prepared for one:
(2), different chicken perfume base sample obtained step (1) carry out the step that headspace gas chromatography-mass spectrophotometry measures, different chicken perfume base sample is carried out in the step of headspace gas chromatography-mass spectrophotometry mensuration at one, first get chicken perfume base sample 8g respectively, ml headspace bottle that sodium chloride 1g puts into 15mL or 20ml, 65 ~ 75 DEG C of water-bath balance 10 ~ 15min, in 65 ~ 75 DEG C of water-baths, SPME head space Static Adsorption 50 ~ 60min; Then by SPME extracting head, the gas chromatographic sample introduction mouth inserted in headspace gas chromatography-GC-MS is resolved, and resolution temperature 230 ~ 250 DEG C, resolves time 5 ~ 8min, different chicken perfume base samples is carried out to the mensuration of volatile ingredient; In described headspace gas chromatography-GC-MS, gas chromatography condition of work is: mm × 0.25 μm, HP-INNOWAX(60 m × 0.25) chromatographic column; Heating schedule: initial temperature is set to 50 DEG C, keeps 2 ~ 4min, with the ramp to 230 DEG C of 4 DEG C/min, maintains 10 ~ 15min; Carrier gas He, flow velocity 1mL/min; Splitless injecting samples; Mass spectrum condition of work: solvent delay 3min, ion source temperature 230 DEG C, EI ionization source, electron energy 70eV, sweep limit 30 ~ 450amu; Again qualitative and quantitative analysis is carried out to the volatile ingredient in chicken perfume base sample, mass spectrometric data in volatile ingredient mensuration process in above-mentioned different chicken perfume base sample mated with 3 standard spectrum storehouses MAINLIB, NISTDEMO, WILLEY in computer chemistry workstation, By consulting literatures retention index carries out qualitative analysis; Carry out quantitative test in conjunction with interior scalar quantity and peak area ratio to mate with 3 standard spectrum storehouses MAINLIB, NISTDEMO, WILLEY in chem workstation, By consulting literatures retention index carries out qualitative analysis;
(3), Dimension Reduction Analysis and cluster analysis is carried out by the different chicken perfume base volatile ingredient qualitative and quantitative analysis results of PCA-HCA to above-mentioned steps (2) gained, in conjunction with sense organ descriptive analysis, subjective fragrance description is carried out to chicken perfume base sample, Flavor analysis is carried out to chicken perfume base, thus chicken perfume base sample is distinguished.
2. a kind of method distinguished chicken perfume base as claimed in claim 1, is characterized in that the step preparing chicken perfume base is as follows:
1) chicken breast meat is taken respectively, deionized water and compound protease, described chicken breast meat, the weight ratio of deionized water and compound protease is 1:3:0.003, and by chicken breast meat, deionized water and compound protease add in a reaction vessel, 45 ~ 55 DEG C of enzymolysis 2 ~ 4h, cooling obtains chicken enzymolysis liquid;
2), take the chicken enzymolysis liquid that step 1) obtains respectively, deionized water, glucose, wood sugar, cysteine salt, glycocoll, alanine, thiamine, salt and monosodium glutamate, described chicken enzymolysis liquid, deionized water, glucose, wood sugar, cysteine salt, glycocoll, alanine, thiamine, the weight ratio of salt and monosodium glutamate is 39:13:1:0.5:1:0.5:0.5:1:3:0.5, by chicken enzymolysis liquid, deionized water, glucose, wood sugar, cysteine salt, glycocoll, alanine, thiamine, salt and monosodium glutamate add in another one reaction vessel, under the condition of pH 7.5 ~ 9.0,105 ~ 110 DEG C of oil bath reaction 0.5 ~ 1.5h obtain chicken perfume base.
3. a kind of method that chicken perfume base is distinguished as claimed in claim 1, it is characterized in that: the aroma volatile in chicken perfume base is being carried out in the step of PCA-HCA analysis, utilize statistical software XLSTAT2010 to carry out PCA and HCA to the aroma substance of qualitative, quantitative in chicken perfume base to analyze, first centralization process and nondimensionalization process are carried out to data, after process, data point carries out PCA Dimension Reduction Analysis according to covariance arithmetic, obtain each data point and the sample distribution plan at first principal component and Second principal component, according to Euclidean distance method and sum of squares of deviations method, HCA cluster analysis is carried out to sample, obtain sample classification figure.
4. a kind of method that chicken perfume base is distinguished as claimed in claim 1, it is characterized in that: described Volatile infochemicals comprises: 2-furfuryl mercaptan, 3-methylpyrrole, 2-acetyl pyrrole, 2-methyl-3-hydroxyl-pyrokomane, 2-methylfuran, 2-amyl furan, 2-methyl-3-sulfydryl furans, 2-acetyl furan, two (2-methyl-3-furyl) disulfide, 3-methylbutyraldehyd, hexanal, aldehyde C-9, 2-octenal, furfural, benzaldehyde, 2-methylthiophene, n-octyl alcohol, pyrazine, thiazole, 4-methylthiazol, 2-acetylthiazole, 4-methyl-5-hydroxy ethylthiazole, 2-methyltetrahydrofuran-3-ketone, methyln-hexyl ketone, 3-sulfydryl-2 pentanone, 2-HEPTANONE, Ergol, formic acid, acetic acid, caproic acid, sad, dodecoic acid, tetradecylic acid and hexadecylic acid.
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| CN106053666A (en) * | 2016-07-14 | 2016-10-26 | 上海应用技术学院 | Method for identifying nitrogen-containing compound in top-frozen oolong tea |
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