CN105241917B - A kind of evaluation method of honey - Google Patents
A kind of evaluation method of honey Download PDFInfo
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Abstract
The present invention relates to food analysis and Safety of Food Quality field, more particularly to a kind of evaluation method of honey, following steps are specifically included：(1) DSC curve of honey need to be detected using differential scanning calorimetry measure, according to the shape of DSC curve, judges to detect whether honey crystallizes；(2) water activity that need to detect honey is determined；(3) as it is described need to detect honey while meet do not crystallize with water activity ＜ 0.6, then need the quality of detection honey good；Need detection honey to be unsatisfactory for one of condition as described, then need to detect the quality decline of honey.The method of the present invention can be with the crystalline state of effective evaluation honey, while the evaluation criterion using water activity as honey microorganism can greatly improve the ageing of detection.
Description
Technical field
The present invention relates to food analysis and Safety of Food Quality field, specifically, is related to a kind of evaluation method of honey.
Background technology
Honey is after gathering nectar or honeydew from the flower of nectariferous plant by honeybee (Apis mellifera L.), is incited somebody to action
It is stored in the honeycomb in honeycomb, is formed through fully brew.Ripe honey is a kind of crude sweet thing with foundation for heavy florals taste
Matter, in all age, eaten extensively by people because it has higher nutritive value.Under normal temperature, honey is translucent sticky
Shape liquid, after low temperature is deposited long, it may appear that partially crystallizable or all crystallization.The crystallization of honey may be with its nectar source species, material group
Into or thermodynamic characteristics etc. it is closely related.
The honey of different crystalline states is produced or evaluated, the product of bright characteristic, Er Qieyou can not only be provided for consumer
Help improve production technology, bigger profit is created for the producer.
The chemical constituent of crystallized honey and noncrystalline honey is more similar, and difference focuses mostly in the physical state of some compositions
Or the change of content, and the Authentic Assessment of honey is extremely important to the right to know of consumer and the credit worthiness of enterprise.From legislation
Angle say that numerous quality tabs on honey need to provide the special of every kind of product it has been established that required according to quality tab
State and important physical feature.Moreover, from economic angle, the high honey of productive consumption person's acceptance, honeybee is such as crystallized
Honey or solid bee honey etc. (referring to the crystallized honey or solid bee honey by special processing), can further improve value-added content of product.
Therefore, it is a technical problem that how science, which illustrates the specific features of honey, and its basic main points is：Utilize certain technological means
The crystalline state of accurate evaluation honey, and ensure the stabilization of its quality.
At present, it is conventional mainly to have three kinds of methods.The first is the content for detecting some special chemical materials, with the proviso that
Assuming that comparision contents of these materials in certain honey are fixed.Theoretically, for the multiplicity of plurality of target material
Method can separate difference sample from specific sample group.However, honey sample is because of acquisition mode, condition of storage and adds
The difference of work technology etc. can cause the content of these target substances to change, and in turn result in the exception of testing result.Also, this
Kind method needs to evaluate each group with stechiometry, principal component analysis, linear discriminant analysis or artificial neural network analysis etc.
Similar or difference degree between data, there is the defects of analysis process is cumbersome, data volume is big in it.
Second method is that a kind of special mark is found in particular state honey, and it can be certain chemical composition
(such as compound, molecule, nucleic acid) or anatomic element (such as plant cell) are to prove the authenticity in honey source.
The third method is the Global Information based on honey, and mainly with physical analysis technology for detection, certain source honey is whole
The physicochemical characteristics of body, rather than a kind of physical and chemical index is only detected, for example pH, electrical conductivity, moisture, ash grade.
Differential scanning amount is a kind of thermal analysis system, is initially used to the physical attribute for analyzing some industrial materials, in material
Scientific domain is widely used.However, the report that simultaneously no-trump differential scanning calorimetry applies in honey detection at present.Specifically,
Differential scanning calorimetry is under programed temperature, and measurement is input to the difference power of sample and reference substance (as in the form of heat)
With the relation of temperature, the curve that differential scanning calorimeter recorded claims DSC curve, and it is with the speed of sample neither endothermic nor exothermic, i.e.,
Rate of heat flow dH/dt (unit MJ/second) is ordinate, using temperature T or time t as abscissa, can determine a variety of thermodynamics and
Kinetic parameter, such as specific heat capacity, reaction heat, the heat of transformation, phasor, reaction rate, crystalline rate, superpolymer crystal degree, sample
Purity etc..The method use temperature range wide (- 175~725 DEG C), high resolution, sample dosage are few.Suitable for inorganic matter, organic
Compound and Pharmaceutical Analysis.
The content of the invention
For the state of easier evaluation honey, and ensure the stability of its quality, it is of the invention by differential scanning amount
Hot method is used in the detection of honey, and by analyzing the relation of honey sample material composition and macroscopic property, there is provided one
The evaluation method of the simple and effective honey of kind.
The relation of honey sample material composition and macroscopic property has been inquired into present invention analysis first, specific method include with
Lower step：
(1) different nectar sources, the honey of different crystalline states are chosen as sample；
(2) moisture, water activity, glucose content, fructose content, the glass transition temperature of the sample are determined
Degree, the gentle endothermic peak enthalpy change in endothermic peak peak；
(3) one-way analysis of variance is carried out to moisture, water activity, glucose content and fructose content；
(4) otherness ratio is carried out to glass transition temperature, the gentle endothermic peak enthalpy change in endothermic peak peak using paired t-test
Compared with；
(5) using Bivariate correlation (two variable correlation analyses) method to moisture, water activity, Portugal
The gentle endothermic peak enthalpy change in grape sugared content, fructose content, glass transition temperature, endothermic peak peak carries out correlation analysis.
In the present invention, nectar source refers mainly to the plant needed for honeybee producting honey, and main nectariferous plant includes Chinese scholartree, jujube tree, chaste tree
The seeds such as bar, lime tree, rape, the geographic area of these plant integrated distributions is with being referred to as nectar source.
Moisture, water activity, glucose content, fructose content, glass transition temperature, endothermic peak in step (2)
The measure of the gentle endothermic peak enthalpy change in peak can use conventional technical means of the prior art, such as moisture to be rolled over using Abbe
Instrument measure is penetrated, water activity is determined using admeasuring apparatus for measuring moisture content of substance, and glucose content and fructose content use liquid chromatogram measuring, glass
Change transition temperature, the gentle endothermic peak enthalpy change in endothermic peak peak is determined using differential scanning calorimetry, and obtains DSC curve.
The step of one-way analysis of variance in step (3) is：With moisture, water activity, glucose content and fruit
Sugared content is observational variable, using four different experiments groups as control variable (crystallization lime tree honey DG, do not crystallize lime tree honey DY,
Acacia honey YG is crystallized, does not crystallize acacia honey YY), determine moisture, water activity, grape of the null hypothesis for four groups of samples
The population mean of sugared content and fructose content difference is equal, and F statistical values are calculated automatically using SPSS softwares, if a certain observation becomes
The Probability p value that accompanies of amount is less than significance 0.05, refuses null hypothesis, it is believed that each population mean of the observational variable has significantly
Difference, on the contrary then on the contrary, i.e. no difference.
Obtained by one-way analysis of variance：In terms of fructose and glucose content, the noncrystalline and crystallization in same nectar source
Honey between there is no difference；And between the honey in different nectar sources there is significance difference in (either crystalline state or non-crystalline)
Different (p<0.05).However, the honey of different nectar sources or different crystalline states, does not have in 2 indexs of moisture and water activity
It is variant.
It is the step of paired t-test in step (4)：Assume initially that the glass of different nectar sources or different crystalline state honey samples
There is no difference between glass transition temperature, endothermic peak peak three variables of gentle endothermic peak enthalpy change, i.e. nectar source or crystalline state is to glass
The gentle endothermic peak enthalpy change in glass transition temperature, endothermic peak peak does not influence；Using SPSS softwares to glass transition temperature, heat absorption
Peak gentle endothermic peak enthalpy change data in peak are handled, and obtain F statistical values, are shown if the Probability p value that accompanies of a certain variable is less than
Work property level 0.05, then refuse to assume, it is believed that there were significant differences for each population mean of the variable, on the contrary then on the contrary, i.e. no difference.
Obtained by step (4)：Obvious glass transition temperature, Er Qiemi be present in either noncrystalline or crystallized honey
The change of source or crystalline state can cause the change of glass transition temperature, and glass transition temperature, endothermic peak enthalpy change and suction
Thermal spike peak temperature can have notable difference between the honey sample of different nectar sources or crystalline state.
The gentle endothermic peak enthalpy change difference in the glass transition temperature of nectar source of the same race but different crystalline state honey, endothermic peak peak
Significantly, the gentle endothermic peak enthalpy change in glass transition temperature, endothermic peak peak of different nectar sources but crystalline state honey of the same race does not have
Difference, illustrating the nectar source of DSC curve and honey does not have obvious correlation, i.e., when crystalline state is identical, the shape of its DSC curve
Shape is similar, therefore can be judged detect whether honey crystallizes according to the shape of DSC curve.
When nectar source difference, difference is mainly reflected in glass transition temperature Tg, endothermic peak peak temperature Tpk and endothermic peak enthalpy change etc.
Data, i.e. Tg, Tpk and Δ H are more sensitive for distinguishing different honey samples, therefore technical scheme is also included into one
The nectar source that the detection honey is judged according to glass transition temperature, the gentle endothermic peak enthalpy change in endothermic peak peak of step.
Therefore, the thermodynamic characteristics of honey are studied using differential canning calorimetry, are expected to not realize to different nectar sources or not
The scientific evaluation of syncrystallization state honey feature and quality.
Step (5) using Bivariate correlation carry out correlation analysis the step of be：Bivariate
Whether point-blank correlation correlation analyses are to be based on measurement two datasets conjunction face, i.e. line between two variables
Sexual intercourse, specific formula for calculation are：
In above-mentioned formula, r representative sample coefficient correlations；X represents the numerical value of first data acquisition system；Y represents second
The numerical value of data acquisition system.
Obtained by step (5)：The material composition of honey and its thermodynamic parameter do not have a significant correlation, i.e. honey
Nectar source feature may influence little on its macroscopic property.
Step (5) using the honey of different nectar sources and different crystalline states as test material, analyze its material composition and
Correlation between macroscopic property, and material composition and macroscopic property.The final water activity and knot for thinking honey
Brilliant degree is relevant with moisture, and the water activity by monitoring honey helps to control the taste of microorganism (especially saccharomycete)
It is raw.Learnt simultaneously through correlation analysis, honey thermodynamic parameter is relevant with its crystalline state, can be turned by determining the glass of honey
Change the indexs such as temperature, the gentle endothermic peak enthalpy change in endothermic peak peak, judge the crystallization degree of honey.Such as it can use and be swept using differential
The DSC curve of honey need to be detected by retouching calorimetry dynamic monitoring, if DSC curve glass transition temperature (Tg) persistently raises, and be inhaled
Thermal spike peak temperature (Tpk) persistently reduces, and heat absorption peak shape tends towards stability, without obvious the lowest point, then need to detect honey it is crystallized or
It will crystallize.
According to above-mentioned conclusion, the invention provides a kind of evaluation method of honey, comprise the following steps：
(1) DSC curve of honey need to be detected using differential scanning calorimetry measure, according to the shape of DSC curve, judges to need
Whether detection honey crystallizes；
(2) water activity that need to detect honey is determined；
(3) as it is described need to detect honey while meet do not crystallize with water activity ＜ 0.6, then need the quality of detection honey good
It is good；Need detection honey to be unsatisfactory for one of condition as described, then need to detect the quality decline of honey.
Specifically, judge that need to detect the specific method whether honey crystallizes is in step (1)：If DSC curve endothermic peak
Shape is precipitous, there is obvious the lowest point, then needs detection honey not crystallize；If DSC curve heat absorption peak shape is gentle, without obvious paddy
Bottom, then need detection honey crystallized.
Preferably, judge that need to detect the specific method whether honey crystallizes is in step (1)：If DSC curve glass turns
It is relatively low to change temperature Tg, and endothermic peak peak temperature Tpk is higher, heat absorption peak shape is precipitous, has obvious the lowest point (as shown in Figure 2), then needs to examine
Honey is surveyed not crystallize；If DSC curve glass transition temperature Tg is higher, and endothermic peak peak temperature Tpk is relatively low, and heat absorption peak shape is put down
It is slow, without obvious the lowest point (as shown in Figure 3), then need detection honey crystallized.
In technical scheme, step (2) can only judge the quality of honey by the numerical value of water activity.Tool
Body, as water activity ＞ 0.60, the growth of microorganism (especially saccharomycete) will be beneficial to.
Specifically, the acquisition condition of DSC curve is in step (1)：5~10mg need to be detected into honey and be sealed in aluminum cup
In, 140~160 DEG C are warming up to from -90~-70 DEG C, the rate of heat addition is 4~6 DEG C/min；Preferably, 150 are warming up to from -80 DEG C
DEG C, the rate of heat addition is 5 DEG C/min.
The assay method of water activity is in step (2)：After admeasuring apparatus for measuring moisture content of substance correction, moisture work is carried out to honey need to be detected
Degree measure, the response of an admeasuring apparatus for measuring moisture content of substance is recorded every 5~6min, when the difference of adjacent response twice is less than 0.005,
As measured value.
The present invention, can be with the crystalline state of effective evaluation honey, while with moisture by detecting the DSC curve of honey sample
Evaluation criterion of the activity as honey microorganism, original microculture detection method is substituted, greatly improves the ageing of detection,
Compared with existing honey evaluation method, there is the characteristics of simple, quick, efficient, with strong points.There is provided furthermore with the present invention
Detection method may determine that, predict shelf life and the storage period of honey, surely effective honey processing and holding conditions are selected in help
Deng being played an important role in the period of processing and storing of honey.
For example, detecting whether honey crystallizes by differential scanning calorimetry, if crystallization illustrates its quality decline, exceed
Shelf life and storage period, reduce commodity value；Water activity by detecting honey judges its microbial infection and fermentation
Degree, such as water activity>0.6, then honey microbial infection and the increased risk of fermentation, shelf life and storage period significantly contracted
It is short.
Brief description of the drawings
Fig. 1 is the analysis of glucose content in honey sample, fructose content, moisture and water activity；
Fig. 2 is the DSC curve of sequence number 2 and the honey sample of sequence number 4；X-axis (Temperature) represents temperature in fig. 2；Y
Axle (Heat Flow) represents heat flux；
Fig. 3 is the DSC curve of sequence number 1 and the honey of sequence number 3；X-axis (Temperature) represents temperature in figure 3；Y-axis
(Heat Flow) represents heat flux；
Fig. 4 is the ratio of glass transition temperature Tg, endothermic peak peak temperature Tpk and endothermic peak enthalpy change in the honey sample of sequence number 1~4
Compared with；
Fig. 5 is the sample similarity analysis based on glass transition temperature Tg, endothermic peak peak temperature Tpk and the peak size that absorbs heat；
Glass Transition temperature represent glass transition temperature, alternatively referred to as glass transition temperature in Fig. 5；
Endothermic peak enthalpy change represent endothermic peak enthalpy change；Endothermic peak temperature tables
Show endothermic peak peak temperature.
Fig. 6 is the correlation analysis based on material composition and thermodynamic parameter.
Embodiment
Following examples are used to illustrate the present invention, but are not limited to the scope of the present invention.
Embodiment 1：The method for inquiring into honey sample material composition and macroscopic property
Honey sample material composition is inquired into the present embodiment and the method for macroscopic property comprises the following steps：
1st, different nectar sources, the honey of different crystalline states are chosen as sample；
2nd, the moisture of the measure honey sample, water activity, glucose content, fructose content, DSC curve, glass
The gentle endothermic peak enthalpy change in glass transition temperature, endothermic peak peak；
3rd, one-way analysis of variance is carried out to moisture, water activity, glucose content and fructose content；
4th, otherness comparison is carried out to glass transition temperature, the gentle endothermic peak enthalpy change in endothermic peak peak using paired t-test；
5th, moisture, water activity, glucose content, fructose are contained using Bivariate correlation methods
The gentle endothermic peak enthalpy change in amount, glass transition temperature, endothermic peak peak carries out correlation analysis.
Now each step is described in detail respectively.
1st, the nectar source of clear and definite honey sample and crystalline state：Honey sample in this experiment picks up from the corresponding nectar source main product in China
Apis mellifera (the Apis mellifera ligustica) bee farm in area, including 2 kinds of nectar sources, 2 kinds of states honey sample (see
Table 1).All samples be nectariferous plant bloom honey flow midseason collection capping honey, the sampling time is in May, 2014~7
Month.Each sampling position is typically populated with the bee-keeping family of more than 10, and the distance between respective more than 5km, cultivates scale one
As be 100 groups or so.Every kind of honey sample parallel acquisition 3 times, 12 samples, each sample sampling quantity are 50g altogether.Non-crystalline
It is sealed at 4 DEG C of honey, the processing mode of crystalline state honey stores more than 6 months for 14 DEG C, to being fully crystallized.Honey sample
The confirmation of nectar source information, the sense organ for relying primarily on interview bee-keeping family, investigation sampled point nectariferous plant species and professional differentiate
Deng.
The honey sample information of table 1
2nd, the moisture of measure honey sample, water activity, glucose content, fructose content, DSC curve, vitrifying
The gentle endothermic peak enthalpy change in transition temperature, endothermic peak peak
(1) water content of Abbe refractometer determination sample is utilized.Sample is coated in refracting prisms surface first, and will enter
Light prism covers, and is locked with handwheel, and the step requires that liquid layer is uniform, full of visual field, bubble-free.Then shadow shield is opened, is closed
Speculum, adjusts eyepiece diopter, makes cross hairs imaging clear, now rotation hand wheel and bright-dark cut is found in eyepiece field of view
Position, then rotation hand wheel makes line of demarcation trimming hand wheel, line of demarcation is located at the center of cross hairs, then fit without any colour
Now show that indicating value is the refractive index of fluid to be measured below eyepiece field of view when rotating condenser.Finally converted using honey moisture
Table (table 2), sample refractive index is converted into moisture.Each sample replication 3 times.
The honey moisture conversion table of table 2
| Refraction index, 20 DEG C | Moisture, % | Refraction index, 20 DEG C | Moisture, % | Refraction index, 20 DEG C | Moisture, % |
| 1.5044 | 13.0 | 1.4935 | 17.2 | 1.4830 | 21.4 |
| 1.5038 | 13.2 | 1.4930 | 17.4 | 1.4825 | 21.6 |
| 1.5033 | 13.4 | 1.4925 | 17.6 | 1.4820 | 21.8 |
| 1.5028 | 13.6 | 1.4920 | 17.8 | 1.4815 | 22.0 |
| 1.5023 | 13.8 | 1.4915 | 18.0 | 1.4810 | 22.2 |
| 1.5018 | 14.0 | 1.4910 | 18.2 | 1.4805 | 22.4 |
| 1.5012 | 14.2 | 1.4905 | 18.4 | 1.4800 | 22.6 |
| 1.5007 | 14.4 | 1.4900 | 18.6 | 1.4795 | 22.8 |
| 1.5002 | 14.6 | 1.4895 | 18.8 | 1.4790 | 23.0 |
| 1.4997 | 14.8 | 1.4890 | 19.0 | 1.4785 | 23.2 |
| 1.4992 | 15.0 | 1.4885 | 19.2 | 1.4780 | 23.4 |
| 1.4987 | 15.2 | 1.4880 | 19.4 | 1.4775 | 23.6 |
| 1.4982 | 15.4 | 1.4875 | 19.6 | 1.4770 | 23.8 |
| 1.4976 | 15.6 | 1.4870 | 19.8 | 1.4765 | 24.0 |
| 1.4971 | 15.8 | 1.4865 | 20.0 | 1.4760 | 24.2 |
| 1.4966 | 16.0 | 1.4860 | 20.2 | 1.4755 | 24.4 |
| 1.4961 | 16.2 | 1.4855 | 20.4 | 1.4750 | 24.6 |
| 1.4956 | 16.4 | 1.4850 | 20.6 | 1.4745 | 24.8 |
| 1.4951 | 16.6 | 1.4845 | 20.8 | 1.4740 | 25.0 |
| 1.4946 | 16.8 | 1.4840 | 21.0 |
| 1.4940 | 17.0 | 1.4835 | 21.2 |
(2) water activity of admeasuring apparatus for measuring moisture content of substance determination sample is utilized.First in 18 DEG C -25 DEG C of temperature, humidity 50%-80%
Under conditions of, admeasuring apparatus for measuring moisture content of substance is corrected using saturation NaCl solution.Then, 5g (being accurate to 0.01g) sample is weighed to put
Enter planchet, carry out water activity detecting.The response of an admeasuring apparatus for measuring moisture content of substance is recorded every 5min, when adjacent response twice
Difference when being less than 0.005, as measured value.After often once being determined, it need to be proofreaded again, same sample replication 3
It is secondary.
(3) glucose and fructose content of liquid chromatogram measuring sample are utilized
A, the preparation of standard stock solution, glucose, fructose standard items 5g, 4g, 1g are weighed respectively, is accurate to 0.0001g,
It is put into 100mL volumetric flasks, adds the dissolving of 60mL water, acetonitrile (chromatographically pure) is settled to volume, shaken up.
B, the preparation of standard working solution, glucose, the fructose standard stock solution to 100mL capacity of different volumes are drawn
In bottle, with acetonitrile and water mixed liquid (volume ratio 40：60) volume is diluted to, is made into glucose, the fructose standard work of various concentrations
Make solution, for drawing standard working curve.
C, the preparation of sample, for noncrystalline sample, stirred with clean glass bar.For crystallized sample, closed
In the case of, warm bath in the water-bath no more than 60 DEG C, concussion are placed in, is stirred evenly after sample all melts, is cooled to room temperature.
D, the weighing and extraction of sample, weighs sample 5g, is accurate to 0.0001g, is placed in 100mL beakers, adds 30mL
Water, stirred to sample and be completely dissolved with glass bar.It is transferred in 100mL volumetric flasks, acetonitrile is settled to volume, shake up (while make
Make two Duplicate Samples and reagent blank sample).Stand in a moment, with 0.45 μm of aperture membrane filtration, (be furnished with to liquid chromatogram and show difference
Refraction detector) sample introduction.The determination step of liquid chromatogram, utilize mobile phase (acetonitrile：Water=70：30, use aperture 0.45 using preceding
μm membrane filtration, ultrasound degassing) after stable 2h, conditioning instrumentation balance, when baseline and smaller Composition distribution display numeral fluctuation,
Can loading measure.Chromatographic condition, chromatographic column, Kromsil nh 2 columns, 4.6 μ m 250mm；Flow velocity 1mL/min；Differential refraction
30 DEG C of detector temperature；The μ L of sample size 10.
The test of the moisture, water activity, glucose content, fructose content of the honey sample of above-mentioned serial number 1~4
As a result shown in table 3.
The moisture of the honey sample of table 3, water activity, glucose content, fructose content
| Sequence number | Moisture (%) | Water activity | Glucose content (%) | Fructose content (%) |
| 1 | 22.6 | 0.626 | 25.9 | 40.9 |
| 2 | 22.8 | 0.648 | 25.4 | 40.1 |
| 3 | 24.0 | 0.697 | 32.1 | 36.7 |
| 4 | 23.8 | 0.677 | 30 | 34.4 |
(4) differential scanning calorimetry measure need to detect the DSC curve of honey, and the vitrifying for further obtaining honey turns
The gentle endothermic peak enthalpy change in temperature, endothermic peak peak
Sample analysis is carried out using function compensation type DSC.Need to carry out DSC temperature using indium and zinc solution standard items before experiment
With the calibration of power, baseline scan is carried out using empty crucible, the heating of instrument or cooling process enter in lasting nitrogen atmosphere
OK.Sample size is 5-10mg, is sealed in aluminum cup (volume is 100 μ L), and the rate of heat addition is 5 DEG C/min, the heating of sample
Scope is -80 DEG C~150 DEG C, and range of temperature is ± 1 DEG C.
Test result is as follows, and wherein Fig. 2 is the DSC curve of the honey sample of sequence number 2 and sequence number 4, and Fig. 3 is sequence number 1 and sequence
The DSC curve of numbers 3 honey sample.The gentle endothermic peak enthalpy change in glass transition temperature, endothermic peak peak is as shown in table 4.
The gentle endothermic peak enthalpy change in glass transition temperature, endothermic peak peak of the honey sample of table 4
| Sequence number | Glass transition temperature (DEG C) | Endothermic peak peak temperature (DEG C) | Endothermic peak enthalpy change (J/g) |
| 1 | -65.06 | 133.56 | -56.64 |
| 2 | -32.07 | 68.33 | -12.95 |
| 3 | -58.14 | 123.75 | -57.66 |
| 4 | -22.63 | 63.4 | -11.63 |
3rd, one-way analysis of variance is carried out to moisture, water activity, glucose content, fructose content
Using moisture, water activity, glucose content and fructose content as observational variable, using four different experiments groups as
Variable is controlled, determines null hypothesis for the overall equal of the moisture of four groups of samples, water activity, glucose content and fructose content
Number is equal respectively, and F statistical values are calculated automatically using SPSS softwares, shows if the Probability p value that accompanies of a certain observational variable is less than
Write property level 0.05, refuse null hypothesis, it is believed that there were significant differences for each population mean of the observational variable, it is on the contrary then on the contrary, be do not have
Difference.
The main matter (moisture, glucose and fructose) being directed in experiment in honey is analyzed, the index bag of detection
Fructose content, glucose content, moisture and water activity are included, is specifically shown in Fig. 1.
In terms of fructose and glucose content, the difference condition between 4 samples is similar.I.e. noncrystalline and crystallization acacia
There is no difference between honey, there is no difference between noncrystalline and crystallization lime tree honey；Either crystalline state, or it is noncrystalline
State, significant difference (p between acacia honey and lime tree honey be present<0.05)；The fructose content of acacia honey is apparently higher than linden
Wood wasp honey (p<0.05), and the glucose content of acacia honey is then significantly lower than lime tree honey (p<0.05).
However, the honey sample of different nectar sources or different crystalline states, does not have in 2 indexs of moisture and water activity
It is variant.Because honey is in the case where water activity is higher than 0.60, beneficial to the growth of saccharomycete, therefore acacia honey, linden are compared
The water activity of wood wasp honey may be more conducive to saccharomycete growth.
There is research to think, the water activity of honey can increase with the intensification of crystallization degree, also occur phase in this research
Like trend, but change unobvious, its reason be probably the moisture of selected honey sample in this research itself it is relatively low and
Caused by honey crystallization degree deficiency.As honey crystallization degree is deepened, its water activity increases therewith, it is easy to more than saccharomycete
The threshold value (water activity ≈ 0.60) of growth, formed and be beneficial to the environment that saccharomycete grows.This is also why to crystallize or hypocrystalline honeybee
Sweet the reason for easily growing saccharomycete, the saccharomycete with resistance to sugared (sugar-tolerant) characteristic can cause the fermentation of honey,
In turn result in honey quality decline.
4th, otherness comparison is carried out to the corresponding data of sample using paired t-test
Assume initially that the glass transition temperature in different nectar sources or different crystalline state honey samples, endothermic peak peak are gently inhaled
There is no difference between three variables such as thermal spike enthalpy change, i.e. nectar source or crystalline state is gentle to glass transition temperature, endothermic peak peak
Endothermic peak enthalpy change does not influence；Glass transition temperature, the gentle endothermic peak enthalpy change data in endothermic peak peak are entered using SPSS softwares
Row processing, obtains F statistical values, if the Probability p value that accompanies of a certain variable is less than significance 0.05, refuse it is assumed that
Think that there were significant differences for each population mean of the variable, on the contrary then on the contrary, i.e. no difference.- 80 it can be seen from Fig. 2 and Fig. 3
DEG C~150 DEG C of excursion in, the DSC curve of crystalline state honey (different nectar sources) of the same race is more similar, and essential difference is
The data such as glass transition temperature Tg, endothermic peak peak temperature Tpk and heat absorption peak size, but difference is smaller.Either non-crystalline, also
It is non-crystalline, the Tg of acacia honey is below lime tree honey, and the Tpk of acacia honey is above lime tree honey.
The DSC curve of nectar source honey (different crystalline states) of the same race then significant difference, such as Tg, Tpk, heat absorption peak size and shape
Shape shows significant difference.
The more obvious parameter of difference is mainly have chosen in DSC experiments to be analyzed, including Tg, Tpk and endothermic peak enthalpy change
ΔH.As seen from Figure 4, the Δ H of crystalline state honey of the same race does not have difference, and the Δ H differences without syncrystallization state honey show
Write (p<0.001)；YG and DG Tg significant differences (0.001 in crystalline state honey of the same race<p<0.01), and YY and DY Tg does not have
Difference, the significant difference (p between different crystalline state honey Tg<0.001)；YY and DY Tpk differences in crystalline state honey of the same race
Significantly (0.001<p<0.01), and YG and DG Tpk does not have difference, the Tpk significant differences (p of different crystalline state honey<
0.001).The partial results illustrate that Tg, Tpk and Δ H are more sensitive for distinguishing different honey samples.With Tg, Tpk and heat absorption
Peak enthalpy change Δ H is as reference axis drawing three-dimensional coordinate diagram (Fig. 5), it can be seen that the thermodynamics of crystalline state honey sample of the same race
Matter is more similar, and it is little with the nectar source relation of honey.
5th, correlation analysis is carried out using Bivariate correlation methods
Point-blank whether Bivariate correlation correlation analyses closed based on measurement two datasets
Linear relationship between face, i.e. two variables, specific formula for calculation are：
As seen from Figure 6, fructose content and water activity (Kendall's tau rank:R=-0.826, n=12, p
=0.001), Δ H and Tpk (Kendall's tau rank:R=-0.983, n=12, p=0.000), Tg and Tpk
(Kendall's tau rank:R=-0.986, n=12, p=0.000) in extremely significantly negatively correlated；Glucose content and fructose
Content (Kendall's tau rank:R=-0.630, n=12, p=0.028) in significantly negatively correlated；Glucose content and water
Divide content (Kendall's tau rank:R=0.828, n=12, p=0.001), Δ H and Tg (Kendall's tau
rank:R=0.966, n=12, p=0.000) it is in notable positive correlation；Obvious correlation is not shown between remaining each parameter
Property.In addition, result above also illustrates, the material composition of honey and its thermodynamic parameter do not have an obvious correlation, i.e. honey
Nectar source feature may influence little on its macroscopic property.
Embodiment 2：The evaluation method of honey
1st, honey need to be detected：Honey need to be detected by taking four kinds of honey conducts of sequence number 1~4, need to detect the information such as table 1 of honey
It is shown, but testing staff and be unaware of any information in table 1, i.e., for testing staff, it is unknown that need to detect honey.
2nd, the method that honey is evaluated in the present embodiment, comprises the following steps：
(1) DSC curve of honey need to be detected using differential scanning calorimetry measure, the acquisition condition of wherein DSC curve is：
5~10mg need to be detected into honey to be sealed in aluminum cup, the rate of heat addition is 5 DEG C/min, the temperature elevating range of sample for -80 DEG C~
150 DEG C, range of temperature be ± 1 DEG C, for the sample of sequence number 2 and sequence number 4, the DSC curve finally given as shown in Fig. 2
As shown in Figure 2, the DSC curve glass transition temperature Tg of sequence number 2 and the sample of sequence number 4 is relatively low, and endothermic peak peak temperature Tpk is higher, heat absorption
Peak shape is precipitous, there is obvious the lowest point, thus can determine whether that sequence number 2 and sequence number 4 need to detect honey and not crystallize；
For the sample of sequence number 1 and sequence number 3, the DSC curve finally given finally given is as shown in figure 3, sequence number 1 and sequence
The glass transition temperature Tg of number 3 samples is higher, and endothermic peak peak temperature Tpk is relatively low, and heat absorption peak shape is gentle, without obvious the lowest point, by
This can determine whether sequence number 1 and sequence number 3 need to detect honey crystallized.
(2) measure need to detect the water activity of honey, and concrete operation step is：After admeasuring apparatus for measuring moisture content of substance correction, to needing to detect
Honey carry out water activity detecting, every 5~6min record an admeasuring apparatus for measuring moisture content of substance response, when adjacent response twice it
When difference is less than 0.005, as measured value, test result are as shown in table 5：
The honey sample water activity of table 5
| Sequence number | Water activity |
| 1 | 0.628 |
| 2 | 0.652 |
| 3 | 0.686 |
| 4 | 0.663 |
(3) test result of step (1) and step (2) is aggregated into table 3, as a result as shown in table 6.
The honey sample Global Information of table 6
| Sequence number | Whether crystallize | Water activity | Quality conditions |
| 1 | Crystallization | 0.628 | Quality decline |
| 2 | It is noncrystalline | 0.652 | Quality decline |
| 3 | Crystallization | 0.686 | Quality decline |
| 4 | It is noncrystalline | 0.663 | Quality decline |
It can be seen from the data in table 6 present invention using thermodynamic parameter and water activity evaluation honey crystallization and
Saccharomycete grows situation, adds the objectivity for weighing honey quality, the artificial subjective error in continuous mode is greatly reduced.It is logical
The evaluation method of honey provided by the invention is crossed, can be with the crystalline state of effective evaluation honey, while honeybee is used as using water activity
The evaluation criterion of sweet microorganism, original microculture detection method is substituted, greatly improves the ageing of detection.
Although above the present invention is described in detail with a general description of the specific embodiments,
On the basis of the present invention, it can be made some modifications or improvements, this will be apparent to those skilled in the art.Cause
This, these modifications or improvements, belong to the scope of protection of present invention without departing from theon the basis of the spirit of the present invention.
Claims (1)
1. a kind of evaluation method of honey, it is characterised in that comprise the following steps：
(1) DSC curve of honey need to be detected using differential scanning calorimetry measure, according to the shape of DSC curve, judgement needs to detect
Whether honey crystallizes；Judgement need to detect the specific method whether honey crystallizes and be：If peak shape of being absorbed heat in DSC curve is precipitous,
There is obvious the lowest point, then need detection honey not crystallize；If peak shape of being absorbed heat in DSC curve is gentle, without obvious the lowest point, then need
It is crystallized to detect honey；The acquisition condition of DSC curve is：5~10mg need to be detected into honey to be sealed in aluminum cup, from-
90~-70 DEG C are warming up to 140~160 DEG C, and the rate of heat addition is 4~6 DEG C/min；
(2) water activity that need to detect honey is determined, the assay method of the water activity is：Admeasuring apparatus for measuring moisture content of substance corrects
Afterwards, water activity detecting is carried out to honey need to be detected, the response of an admeasuring apparatus for measuring moisture content of substance is recorded every 5~6min, when adjacent
When the difference of response is less than 0.005 twice, as measured value；
(3) as it is described need to detect honey while meet do not crystallize with water activity ＜ 0.6, then need the quality of detection honey good；
Need detection honey to be unsatisfactory for one of condition as described, then need to detect the quality decline of honey.
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| Crystallization in "Tarassaco" Italian honey studied by DSC;Elena Venir et al.;《Food Chemistry》;20100915;第122卷(第2期);第410-415页，参见摘要、第1、2.1、2.7-2.8、3.2、4部分 * |
| 差示扫描量热法(DSC)是检测蜂蜜掺假的一项新技术;黄文诚;《中国蜂业》;20071105;第58卷(第9期);第33-34页 * |
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