CN102590256B - Method for evaluating flavor stability of beer - Google Patents
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- 235000013405 beer Nutrition 0.000 title claims abstract description 112
- 239000000796 flavoring agent Substances 0.000 title claims abstract description 51
- 235000019634 flavors Nutrition 0.000 title claims abstract description 51
- 238000000034 method Methods 0.000 title claims abstract description 23
- 230000032683 aging Effects 0.000 claims abstract description 38
- HYBBIBNJHNGZAN-UHFFFAOYSA-N furfural Chemical compound O=CC1=CC=CO1 HYBBIBNJHNGZAN-UHFFFAOYSA-N 0.000 claims abstract description 36
- DTUQWGWMVIHBKE-UHFFFAOYSA-N phenylacetaldehyde Chemical compound O=CCC1=CC=CC=C1 DTUQWGWMVIHBKE-UHFFFAOYSA-N 0.000 claims abstract description 36
- 238000011156 evaluation Methods 0.000 claims abstract description 31
- CLUWOWRTHNNBBU-UHFFFAOYSA-N 3-methylthiopropanal Chemical compound CSCCC=O CLUWOWRTHNNBBU-UHFFFAOYSA-N 0.000 claims abstract description 19
- 229940100595 phenylacetaldehyde Drugs 0.000 claims abstract description 18
- 230000001953 sensory effect Effects 0.000 claims abstract description 16
- 238000001514 detection method Methods 0.000 claims abstract description 4
- -1 trans-2-nonenyl aldehyde Chemical class 0.000 claims description 16
- 239000012458 free base Substances 0.000 claims description 14
- 239000000463 material Substances 0.000 claims description 13
- 238000007872 degassing Methods 0.000 claims description 9
- 238000000605 extraction Methods 0.000 claims description 9
- 238000004458 analytical method Methods 0.000 claims description 6
- 238000001212 derivatisation Methods 0.000 claims description 6
- 238000012360 testing method Methods 0.000 claims description 6
- 238000004435 EPR spectroscopy Methods 0.000 claims description 5
- 150000001875 compounds Chemical class 0.000 claims description 4
- 230000000694 effects Effects 0.000 claims description 4
- 238000002290 gas chromatography-mass spectrometry Methods 0.000 claims description 3
- 239000007788 liquid Substances 0.000 claims description 3
- 238000001819 mass spectrum Methods 0.000 claims description 3
- 238000003672 processing method Methods 0.000 claims description 3
- 239000013076 target substance Substances 0.000 claims description 3
- 125000000999 tert-butyl group Chemical group [H]C([H])([H])C(*)(C([H])([H])[H])C([H])([H])[H] 0.000 claims description 3
- 238000012549 training Methods 0.000 claims description 2
- 238000003556 assay Methods 0.000 claims 2
- 238000006243 chemical reaction Methods 0.000 abstract description 13
- 150000003254 radicals Chemical class 0.000 abstract description 7
- 238000013124 brewing process Methods 0.000 abstract description 6
- BSAIUMLZVGUGKX-BQYQJAHWSA-N (E)-non-2-enal Chemical compound CCCCCC\C=C\C=O BSAIUMLZVGUGKX-BQYQJAHWSA-N 0.000 abstract description 4
- 150000001413 amino acids Chemical class 0.000 abstract description 4
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 abstract description 4
- 229910052760 oxygen Inorganic materials 0.000 abstract description 4
- 239000001301 oxygen Substances 0.000 abstract description 4
- 239000000126 substance Substances 0.000 abstract description 4
- 239000002994 raw material Substances 0.000 abstract description 3
- 238000004890 malting Methods 0.000 abstract 1
- 238000013139 quantization Methods 0.000 abstract 1
- 150000002500 ions Chemical class 0.000 description 4
- 230000007246 mechanism Effects 0.000 description 3
- 241000209140 Triticum Species 0.000 description 2
- 235000021307 Triticum Nutrition 0.000 description 2
- 230000003078 antioxidant effect Effects 0.000 description 2
- 238000013459 approach Methods 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- OTEKOJQFKOIXMU-UHFFFAOYSA-N 1,4-bis(trichloromethyl)benzene Chemical compound ClC(Cl)(Cl)C1=CC=C(C(Cl)(Cl)Cl)C=C1 OTEKOJQFKOIXMU-UHFFFAOYSA-N 0.000 description 1
- 150000001299 aldehydes Chemical class 0.000 description 1
- 230000003064 anti-oxidating effect Effects 0.000 description 1
- 238000005842 biochemical reaction Methods 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 238000010219 correlation analysis Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 229940042795 hydrazides for tuberculosis treatment Drugs 0.000 description 1
- 238000011835 investigation Methods 0.000 description 1
- 150000002632 lipids Chemical class 0.000 description 1
- BIZMUZUXEATCLA-UHFFFAOYSA-N n-[(2,3,4,5,6-pentafluorophenyl)methyl]hydroxylamine Chemical group ONCC1=C(F)C(F)=C(F)C(F)=C1F BIZMUZUXEATCLA-UHFFFAOYSA-N 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- HNBFUFIYQWYCDM-UHFFFAOYSA-N oxygen(2-) sulfane titanium(4+) Chemical compound [O--].[O--].S.[Ti+4] HNBFUFIYQWYCDM-UHFFFAOYSA-N 0.000 description 1
- 238000004451 qualitative analysis Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
Abstract
The invention discloses a method for evaluating the flavor stability of beer. Evaluation indexes of the flavor stability of the beer cover the expression of a series of indexes which can reflect the flavor stability of beer, namely free radicals for reflecting the aging violent degree of the beer, furfural for reflecting thermal loads in the brewing process, 3-(methylthio)propionaldehyde for reflecting the control level of amino acid in the malting process, phenylacetaldehyde for reflecting oxygen loads in the brewing process and trans-2-nonenal for reflecting the fresh degree of raw materials. Compared with single indexes, a flavor stability index (FSI) is a relatively high evaluation index for beer at different aging stages and beer of different qualities and brands. The FSI index for reflecting the flavor stability of the beer is comprehensively refined from an angle of free radical chain reactions covering most of aging reactions in the beer and an angle of a key aging substance influencing the flavor of the beer. The index avoids the one-sidedness of single detection indexes, can intuitively and effectively reflect the flavor stability of the beer, and overcomes the disadvantages of subjectivity and unavailable quantization which are caused by sensory evaluation.
Description
Technical field
The invention belongs to beer quality and evaluate field, specifically, relate to a kind of by quantitatively detecting each index in the middle of beer and analyze, thus to the method that beer flavor stability is evaluated.
Background technology
The local flavor of finished beer can occur to change slowly thus affect the flavor stability of beer in storage process.Because the flavor substance in beer relate to chemistry and the biochemical reaction of over one hundred kind of compound, at present mainly sensory evaluation is relied on to the judgement of beer flavor stability, and sensory evaluation also exists subjectivity and can only the defect such as qualitative analysis.
In the research of beer flavor stability in the past, mainly for the aging material of a certain class or a certain agine mechaism, propose the flavor stability that certain single indicative material carrys out evaluating beer, there is stronger limitation.Such as by weighing hydroxyl compound value, the bitter hydrazides value of hexichol, the beer total antioxidation value, LagTime value, titanium dioxide sulfur number etc. that utilize chemical resistance hydrochlorate to measure for object of reference, weigh the freshness of beer or perhaps the flavor stability of beer.But neither one is comprehensively weighed and the method that judges or standard, and therefore its result judged is often not accurate enough.
The reaction affecting beer flavor stability is caused by a series of net reaction caused by free radical, and the aging material simultaneously in beer also has negative effect to local flavor.The invention provides a kind of method of the new evaluating beer flavor stability based on free radical in beer and aging material.
Summary of the invention
The object of the invention is to existing beer flavor stability determination methods not accurate enough, comprehensively cannot weigh various material in beer and, on the deficiency of the impact of stability, provide a kind of method of novel evaluating beer flavor stability.
Technical solution of the present invention is: a kind of evaluation method of beer flavor stability, is made up of following steps:
(1) free base value A, LagTime value B in beer, concentration ppb value C, the 3-methylthiopropionaldehyde concentration ppb value D of furfural, the concentration ppb value E of phenylacetaldehyde and the concentration ppb value F of anti-2-nonenyl aldehyde is measured respectively.
(2) by following formulae discovery flavor stability evaluation number FSI:FSI=(-0.349) * (A-32000)/32000+0.392* (B-120)/120+ (0.373) * (C-70)/70+ (-0.228) * (D-3.5)/3.5+ (-0.317) * (E-15)/15+ (-0.102) * (F-0.16)/0.16.
(3) according to the flavor stability of this FSI value evaluating beer, wherein: when FSI index is greater than 0.3, judge that beer is fresh; When FSI index is between-0.8 to 0.3, beer is in general ageing state; When FSI index is less than-0.8, beer serious aging.
Further, as preferably, adopt and measure free base value in beer and LagTime value with the following method: beer is through centrifugal degasification.Get 9.5ml degasification beer in brown sample bottle, add 0.5ml 1mol/L PBN (the N-tert-butyl group-α-phenyinitrone) ethanolic solution, vortex vortex mixer accelerates mixing.Detection ordering and call method are set with Bruker ELBA for e-scan, detect.ESR (electron spin resonance) condition: mechanical bath temperature: 60 DEG C; Central magnetic field: 3465G; Sweep length: 20G; Microwave power: 4.33MW; Enlargement factor: 2.51*102; Modulating frequency: 86kHz; Modulation amplitude: 2.0G; Times of collection: 4times; Data processing method: S matching.Free-radical contents is directly obtained by instrument, and LagTime value is formed after S matching.
As preferably, adopt the furfural content, 3-methylthiopropionaldehyde concentration, phenylacetaldehyde concentration and the trans-2-nonenyl aldehyde concentration that measure with the following method in beer: get degasification beer 5ml, add 2gNaCl, after On-chip derivatization extraction, direct injected is to gas chromatograph-mass spectrometer analysis, obtains the concentration of each target substance.Wherein On-chip derivatization extraction conditions is: derivative liquid, 60ppmPFBOA (adjacent pentafluoro-benzyl azanol); Extracting head material, 65 μm of PDMS-DVB; Extraction conditions, 50 DEG C of 60min.Compounds GC-MS testing conditions is: DB-5 MS capillary analysis post; Temperature programme, initial temperature 60 DEG C, stops 2min, 5 DEG C/min to 180 DEG C, 1 DEG C/min to 190 DEG C, 30 DEG C/min to 250 DEG C, stops 3min; Mass spectrum selects single ion scan: Selective ion mode is 61,181.
Effective effect of the present invention is: the beer flavor stability evaluation number (Flavor StabilityIndex) that the present invention proposes, i.e. FSI index, combines the expression of a series of indexs that can reflect beer flavor stability: the phenylacetaldehyde of oxygen load and the trans-2-nonenyl aldehyde of reflection raw material freshness in the free radical of reflection beer aging severe degree, the furfural reflecting thermal load in brewing process, the 3-methylthiopropionaldehyde reflecting amino acid level of control in wheat process processed, reflection brewing process.Compared with single index, the beer of FSI exponent pair different ageing step, different quality, different brands is all an evaluation index relatively preferably.From containing the free chain reaction angle of most of aging reaction beer and affecting the aging material angle of key of beer flavor, comprehensively refine the FSI index of reaction beer flavor stability.This index avoids the one-sidedness of single Testing index, intuitively effectively can react the flavor stability of beer, compensate for subjectivity and not energetic defect that sensory evaluation brings.
Embodiment
Finished beer is after storage, and the flavor substance that a series of chain reaction caused by free radical produces brings staling flavour to beer, affects the flavor stability of beer.Along with in recent years to the further investigation of beer flavor stability, there is new understanding to the reaction mechanism of beer aging and the influence mode of aging material to local flavor.
The major part reaction of beer in storage process is relevant with free radical, and in beer, free-radical contents can reflect the severe degree of aging reaction in beer.Detect the free-radical contents in finished beer, content is higher, and show that the aging reaction Shaoxing opera carried out in beer is strong, degree of aging is higher.Meanwhile, for the difference of the endogenous anti-oxidative content of material existed in beer, using LagTime as the foundation judging beer endogenous anti-oxidative ability.
The aging material that beer produces in ageing process has direct impact to beer flavor, and different aging materials reflects the technical controlling difference in Process of Beer Brewing.Wherein, furfural is as the indicator of thermal load, and the thermal load reflected in brewing process controls; 3-methylthiopropionaldehyde belongs to streck aldehyde, i.e. the product of amino acid degradation, reflects the amino acid level of control in wheat process processed; Phenylacetaldehyde is oxygen load indicator, and the dissolved oxygen in reflection brewing process controls; Trans-2-nonenyl aldehyde is the product of lipid oxidation, indirectly reflects the freshness of raw material.Simultaneously 3-methylthiopropionaldehyde and trans-2-nonenyl aldehyde create direct negative effect to beer flavor because of its extremely low threshold value.
In view of reaction mechanisms different in beer storage process and approach, select free-radical contents, LagTime value, furfural content, 3-methylthiopropionaldehyde content, phenylacetaldehyde content and trans-2-nonenal content in beer as the representative index of differential responses approach and mechanism, establish beer flavor stability evaluation number.
Steps of the method are:
1. collect beer sample 90, place 1 week under 35 degree, carry out aging.
2. measure the free base value A in aging beer and LagTime value B:
Beer is through centrifugal degasification.Get 9.5ml degasification beer in brown sample bottle, add 0.5ml 1mol/L PBN (the N-tert-butyl group-α-phenyinitrone) ethanolic solution, vortex vortex mixer accelerates mixing.Detection ordering and call method are set with Bruker ELBA for e-scan, detect.ESR (electron spin resonance) condition: mechanical bath temperature: 60 DEG C; Central magnetic field: 3465G; Sweep length: 20G; Microwave power: 4.33MW; Enlargement factor: 2.51*102; Modulating frequency: 86kHz; Modulation amplitude: 2.0G; Times of collection: 4times; Data processing method: S matching.Free-radical contents is directly obtained by instrument, and LagTime value is formed after S matching.
3. measure the furfural content ppb value C in aging beer, 3-methylthiopropionaldehyde concentration ppb value D, phenylacetaldehyde concentration ppb value E and trans-2-nonenyl aldehyde concentration ppb value F:
Get degasification beer 5ml, add 2gNaCl, after On-chip derivatization extraction, direct injected is to gas chromatograph-mass spectrometer analysis, obtains the concentration of each target substance.Wherein On-chip derivatization extraction conditions is: derivative liquid, 60ppmPFBOA (o-pentafluoro-benzyl azanol); Extracting head material, 65 μm of PDMS-DVB; Extraction conditions, 50 DEG C of 60min.Compounds GC-MS testing conditions is: DB-5MS capillary analysis post; Temperature programme, initial temperature 60 DEG C, stops 2min, 5 DEG C/min to 180 DEG C, 1 DEG C/min to 190 DEG C, 30 DEG C/min to 250 DEG C, stops 3min; Mass spectrum selects single ion scan: Selective ion mode is 61,181.
4. judge the freshness score of beer
The personnel selecting multidigit (more than 6) to be subject to specialty to judge training carry out sensory evaluation to sample, obtain the freshness score of sample.Freshness score is given a mark according to ten point system, and score value is higher, and the freshness of sample is better, and namely flavor stability is better.The freshness score of sample gets all mean value judging judging panel.The freshness of beer is divided into Three Estate by score, and grade classification is in table 1.
Table 1 beer freshness Comment on Standard (ten point system)
5. calculate beer flavor stability evaluation number
Select the beer sample that freshness score is greater than 6.6 points, calculate the mean value of free base value A, LagTime value B, furfural content ppb value C in sample, 3-methylthiopropionaldehyde concentration ppb value D, phenylacetaldehyde concentration ppb value E and trans-2-nonenyl aldehyde concentration ppb value F, determine the distribution range of single index in fresh sample.Wherein free base value A≤32000 in fresh sample; LagTime value B >=120min; Furfural content ppb value C≤70ppb; 3-methylthiopropionaldehyde concentration ppb value D≤3.5ppb; Phenylacetaldehyde concentration ppb value E≤15ppb; Trans-2-nonenyl aldehyde concentration ppb value F≤0.16ppb.
Analyze A, B, C, D, E, F value of each sample, and do correlation analysis with freshness score, obtain related coefficient.Beer flavor stability evaluation number FSI=(-0.349) × (A-32000)/32000+0.392* (B-120)/120+ (-0.373) × (C 70)/70+ (0.228) × (D-3.5)/3.5+ (0.317) × (E-15)/15+ (-0.102) × (F 0.16)/0.16 will be tried to achieve after each index weighting.
According to the testing result of sample, FSI is larger, and freshness is higher, and the flavor stability of beer is better.Situation is judged according to what collect sample, the freshness of beer is divided into Three Estate: fresh, general aging, serious aging, the sensory evaluation score of its correspondence is respectively: > 6.6,6.6-5.5, < 5.5.The judgment criteria of beer flavor stability evaluation number FSI and beer freshness is in table 2.
Table 2 beer flavor stability evaluation number FSI judgment criteria
When FSI index is greater than 0.3, judge that beer is fresh; When FSI index is between-0.8 to 0.3, beer is in general ageing state; When FSI index is less than-0.8, beer serious aging.
Embodiment 1
Finished beer A, certain draft beer is buied in market, detect corresponding index to be respectively: free base value A=28745, LagTime value B=123min, furfural content ppb value C=60.45ppb, 3-methylthiopropionaldehyde concentration ppb value D=2.09ppb, phenylacetaldehyde concentration ppb value E=6.59ppb, trans-2 nonenyl aldehyde concentration ppb value F=0.10ppb.Calculating FSI index is 0.403, according to appraisement system, is judged to be fresh.The sensory evaluation of this sample is equally divided into 7.2 points, is in young beer sensory evaluation fraction range.FSI index assessment result is consistent with sensory evaluation.
Embodiment 2
Finished beer B, certain ordinary beer is buied in market, detect corresponding index to be respectively: free base value A=28860, LagTime value B=105min, furfural content ppb value C=76.30ppb, 3-methylthiopropionaldehyde concentration ppb value D=4.95ppb, phenylacetaldehyde concentration ppb value E=30.52ppb, trans-2-nonenyl aldehyde concentration ppb value F=0.17ppb.Calculating FSI index is-0.477, according to appraisement system, is judged to be generally aging.The sensory evaluation of this sample is equally divided into 6.25 points, is in general aging beer sensory evaluation fraction range.FSI index assessment result is consistent with sensory evaluation.
Embodiment 3
Finished beer C, certain ordinary beer is buied in market, detect corresponding index to be respectively: free base value A=84121, LagTime value B=24min, furfural content ppb value C=35652ppb, 3-methylthiopropionaldehyde concentration ppb value D=18.60ppb, phenylacetaldehyde concentration ppb value E=125.25ppb, anti-2-nonenyl aldehyde concentration ppb value F=0.31ppb.Calculating FSI index is-1.49, according to appraisement system, is judged to be serious aging.The sensory evaluation of this sample is equally divided into 5.30 points, is in serious aging beer sensory evaluation fraction range.FSI index assessment result is consistent with sensory evaluation.
Claims (1)
1. an evaluation method for beer flavor stability, is characterized in that, described method step is as follows:
1) beer flavor stability evaluation number is calculated
Select the personnel being subject to specialty to judge training more than 6 to carry out sensory evaluation to sample, obtain the freshness score of sample; Freshness score is given a mark according to ten point system, and score value is higher, and the freshness of sample is better, and namely flavor stability is better, and the freshness score of sample gets all mean value judging judging panel;
2) the beer sample selecting freshness score to be greater than 6.6 points, calculate the mean value of free base value A, LagTime value B, furfural content ppb value C in sample, 3-methylthiopropionaldehyde concentration ppb value D, phenylacetaldehyde concentration ppb value E and trans-2-nonenyl aldehyde concentration ppb value F, according to the distribution range of index single in fresh sample, determine the reference value of each index, and the positive and negative impact effect to flavor stability, finally determine free base value A≤32000 in fresh sample; LagTime value B >=120min; Furfural content ppb value C≤70ppb; 3-methylthiopropionaldehyde concentration ppb value D≤3.5ppb; Phenylacetaldehyde concentration ppb value E≤15ppb; Trans-2-nonenyl aldehyde concentration ppb value F≤0.16ppb;
3) according to data results, determine the affecting parameters value of the furfural content ppb value C in free base value A, LagTime value B, aging beer, 3-methylthiopropionaldehyde concentration ppb value D, phenylacetaldehyde concentration ppb value E, each numerical value of trans-2-nonenyl aldehyde concentration ppb value F, wherein free base value A for-0.349, LagTime value B is 0.392, furfural content ppb value C is-0.373,3-methylthiopropionaldehyde concentration ppb value D is-0.228, phenylacetaldehyde concentration ppb value E be-0.317 and trans-2-nonenyl aldehyde concentration ppb value F be-0.102;
4) formula F SI=(-0.349) * (A-32000)/32000+0.392* (B-120)/120+ (-0.373) * (C-70)/70+ (-0.228) * (D-3.5)/3.5+ (-0.317) * (E-15)/15+ (-0.102) * (F-0.16)/0.16 is substituted into;
FSI is larger, and freshness is higher, and the flavor stability of beer is better, when FSI index is greater than 0.3, judges that beer is fresh; When FSI index is between-0.8 to 0.3, beer is in general ageing state; When FSI index is less than-0.8, beer serious aging;
5) evaluation procedure: collect beer sample, place 1 week under 35 degree, carry out aging, measure the furfural content ppb value C in free base value A, LagTime value B in aging beer, aging beer, 3-methylthiopropionaldehyde concentration ppb value D, phenylacetaldehyde concentration ppb value E and trans-2-nonenyl aldehyde concentration ppb value F subsequently;
The assay method of free base value A and LagTime value B is: beer is through centrifugal degasification, get 9.5ml degasification beer in brown sample bottle, add the ethanolic solution of the 0.5ml 1mol/L N-tert-butyl group-α-phenyinitrone, vortex vortex mixer accelerates mixing, detection ordering and call method are set with Bruker ELBA for e-scan, detect; Electron spin resonance condition: mechanical bath temperature: 60 DEG C; Central magnetic field: 3465G; Sweep length: 20G; Microwave power: 4.33MW; Enlargement factor: 2.51*102; Modulating frequency: 86kHz; Modulation amplitude: 2.0G; Times of collection: 4times; Data processing method: S matching free-radical contents is directly obtained by instrument, and LagTime value B is formed after S matching;
The assay method of furfural content ppb value C, 3-methylthiopropionaldehyde concentration ppb value D, phenylacetaldehyde concentration ppb value E and trans-2-nonenyl aldehyde concentration ppb value F comprises the following steps: get degasification beer 5ml, add 2gNaCl, after On-chip derivatization extraction, direct injected is to gas chromatograph-mass spectrometer analysis, obtains the concentration of each target substance; Wherein On-chip derivatization extraction conditions is: derivative liquid, the o-pentafluoro-benzyl azanol of 60ppm; Extracting head material, 65 μm of PDMS-DVB; Extraction conditions, 50 DEG C of 60min; Compounds GC-MS testing conditions is: DB-5MS capillary analysis post; Temperature programme, initial temperature 60 DEG C, stops 2min, 5 DEG C/min to 180 DEG C, 1 DEG C/min to 190 DEG C, 30 DEG C/min to 250 DEG C, stops 3min; Mass spectrum selects single ion scan: Selective ion mode is 61,181;
6) substitute into formulae discovery according to testing result, utilize result of calculation assess sample flavor stability.
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| CN106405024B (en) * | 2016-08-25 | 2018-08-24 | 青岛啤酒股份有限公司 | A method of evaluation malt lipid oxidation degree |
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| CN111398524B (en) * | 2020-04-01 | 2022-10-04 | 北京燕京啤酒股份有限公司 | Identification threshold value of key flavor components of beer and evaluation method of harmony of key flavor components of beer and hop aroma |
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| CN101285763A (en) * | 2008-05-16 | 2008-10-15 | 江南大学 | Beer aging evaluation method |
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