CN103278573B - Method for identifying rape honey and vervain family honey - Google Patents
Method for identifying rape honey and vervain family honey Download PDFInfo
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- CN103278573B CN103278573B CN201310148946.8A CN201310148946A CN103278573B CN 103278573 B CN103278573 B CN 103278573B CN 201310148946 A CN201310148946 A CN 201310148946A CN 103278573 B CN103278573 B CN 103278573B
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Abstract
The invention discloses a method for identifying rape honey and vervain family honey. The method is characterized by comprising the following steps of 1, constructing an identification model by treating provided samples of rape honey and vervain family honey, determining content of amino acids obtained by honey protein hydrolysis, wherein the number of each kind of the samples is greater than or equal to 15, setting Y variables as classified variables, setting values of the Y variables of rape honey and vervain family honey respectively as 0 and 1, setting a threshold value as 0.5, carrying out linear regression of the determined amino acid content and the classified variables of the samples by a partial least square discriminant analysis method, and building the identification model, and 2, carrying out identification by treating honey needing to be identified, determining content of amino acids obtained by honey protein hydrolysis, carrying out identification by the identification model obtained by the step 1 according to the determined amino acid content, and determining if the identified honey belongs to rape honey or vervain family honey. The method can effectively identify rape honey and vervain family honey.
Description
Technical field
The present invention relates to a kind of discrimination method of honey, be specifically related to the discrimination method of a kind of rape honey and chaste honey.
Background technology
Honey, as a kind of natural source health products and nutriment, is subject to consumers in general's favor deeply, but along with improving constantly that people realize Product quality and safety, requires manufacturer to indicate the source of honey, especially plant source, the i.e. title of nectariferous plant.Aspect mouthfeel, smell, color and luster and nutritional labeling, there is notable difference in the honey of different nectariferous plants, some illegal manufacturers are due to the trend of interests, can adulterate, mix the spurious with the genuine, therefore need effective, the reliable method of exploitation to differentiate the plant source kind of honey.
Although there are some differences aspect color and luster, smell in the honey of different nectariferous plants, but be difficult to distinguish discriminating by these proterties, the method of ripe discriminating honey plant source is pollen cell analysis in honey relatively at present, but this method requires high to testing staff's technical merit, and inapplicable to some honey, because in honey corresponding plants pollen amount number with put honeybee environment and have direct relation, put honeybee point and be positioned at this plant distributive province, on the occasion of the flower pesticide phase, this plant pollen percent content is just high again; If it is far away or outside the florescence, this plant pollen content is just low apart from this plant distributive province to put honeybee point.
As pollen alternative method, existing bibliographical information adopts different instrument analysis technologies, by measuring the tagged compound of different nectariferous plants in honey, realizes discriminating.In " research of the qualitative discriminating honey types of near-infrared spectrum technique and the true and false " literary composition of " modern food science and technology " o. 11th in 2010, disclose the method that gathers and set up data model and differentiate sophorae honey, rape honey and chaste honey by infrared spectrum, differentiated accuracy and reached 89.69%.The method need to adopt the instrument and equipments such as Fourier Transform Near Infrared instrument, differentiates that cost is high, complicated operation, and meanwhile, the dependence that identification result is set up for model is higher.
Therefore, need to provide a kind of more convenient, discrimination method accurately.
Summary of the invention
Goal of the invention of the present invention is to provide the discrimination method of a kind of rape honey and chaste honey, to improve the accuracy of discriminating.
To achieve the above object of the invention, the technical solution used in the present invention is: the discrimination method of a kind of rape honey and chaste honey, comprises the following steps:
(1) build and differentiate model:
Sample to the rape honey providing in advance and chaste honey is processed, and measures honey protein hydrolytic amino acid, and the sample number of every kind of honey is no less than 15;
Y variable is made as to classified variable, the Y variate-value of chaste honey and rape honey is set as respectively 0 and 1, Threshold is 0.5, adopts partial least squares discriminant analysis method (PLS-DA) that the amino acid content in the sample recording and classified variable are carried out to linear regression, sets up and differentiates model;
(2) differentiate:
Honey to be identified is processed, measured honey protein hydrolytic amino acid, according to the amino acid content recording, the discriminating model that utilizes step (1) to obtain is differentiated, determines that honey to be identified belongs to chaste honey or rape honey.
In technique scheme, the assay method of honey protein hydrolytic amino acid comprises the following steps:
1. the water that adds 2～3 times of volumes in honey, mixes, and gets supernatant after centrifugal treating;
2. adopt the 1. middle supernatant obtaining of trichloroacetic acid freezing treatment step, obtain honey albumen precipitation;
3. honey albumen precipitation is transferred in hydrolysis pipe to acid hydrolysis honey albumen under vacuum condition with hydrochloric acid solution;
4. adopt automatic amino acid analyser to measure honey protein hydrolytic amino acid.
Step 1. in, centrifugal treating is at 1500g, under 4 DEG C of conditions, centrifugal 10min.
Step 2. in, trichloroacetic acid freezing is specially, in supernatant, add 50%～100% the trichloroacetic acid that is equivalent to honey volume, fully mix, after-20 DEG C of placement 15min, then place 1h in 4 DEG C, make the albumen precipitation in honey, by centrifuge tube in 4 DEG C, centrifugal 10min under 10000g condition, abandoning supernatant.
Step concrete grammar is 3., the hydrochloric acid solution of employing 6.0mol/L divides to be transferred to albumen precipitation in hydrolysis pipe for three times completely, be filled with after nitrogen, be evacuated to vacuum with vacuum pump, will hydrolysis channel closure and be hydrolyzed 24h in the thermostatic drying chamber of 110 DEG C, take out to be cooled to room temperature, by the common Filter paper filtering of hydrolyzate, filtrate nitrogen at 50 DEG C dries up, and finally residue is used to 0.02mol/L dissolve with hydrochloric acid solution, 0.25 μ m water system membrane filtration, obtains testing sample.
Preferred technical scheme, at least measures following 15 seed amino acid content, Asp, Thr, Ser, Glu, Gly, Ala, Val, Ile, Leu, Tyr, Phe, Lys, His, Arg, Pro.
Because technique scheme is used, the present invention compared with prior art has following advantages:
1. the present invention adopts PLS-DA techniques of discriminant analysis that the amino acid content in the honey sample recording and classified variable are carried out to linear regression, to 39 of calibration set honey Sample Establishing discrimination models, total differentiation rate is 92.3%, the calibration model that utilizes PLS-DA method to set up, 17 samples that have neither part nor lot in modeling are carried out to check analysis, total differentiation rate is 94.1%, is a kind of method of effective discriminating rape honey and chaste honey.
2. the present invention, by the extraction step of honey albumen, has removed pollen, has avoided the impact of pollen particles on identification result.
Brief description of the drawings
Fig. 1 is the relation of concentrating between chaste honey and PLS predicted value and the measured value of rape honey sample classification variable of proofreading and correct in embodiment;
Fig. 2 is that the relation between chaste honey and PLS predicted value and the measured value of rape honey sample classification variable is concentrated in checking.
Embodiment
Below in conjunction with drawings and Examples, the invention will be further described:
Embodiment mono-: the discrimination method of rape honey and chaste honey, comprises the following steps:
1) extraction of honey albumen and hydrolysis: accurately take 10.0g (being accurate to 0.01g) honey sample in 50mL centrifuge tube, add 20mL water, mix, with 1500g, 4 DEG C of centrifugal 10min, remove bottom pollen granule, and supernatant is transferred in another centrifuge tube.In supernatant, add 4mL 100% trichloroacetic acid, fully mix, after-20 DEG C of placement 15min, then in 4 DEG C of placement 1h, make the albumen precipitation in honey.By centrifuge tube in 4 DEG C, centrifugal 10min under 10000g condition, after abandoning supernatant, by the albumen precipitation 3mL of bottom, the hydrochloric acid solution of 3mL and 4mL6.0mol/L divides to be transferred to for three times in hydrolysis pipe completely, be filled with after nitrogen, be evacuated to vacuum with vacuum pump, will hydrolysis channel closure and be hydrolyzed 24h in the thermostatic drying chamber of 110 DEG C, take out, to be cooled causing after room temperature, by hydrolyzate with common Filter paper filtering in 50mL volumetric flask, ultrapure water rinses filter paper and is also settled to scale.Draw 1mL filtrate in glass tube, nitrogen dries up at 50 DEG C, finally residue is used to 0.02mol/L dissolve with hydrochloric acid solution, and 0.25 μ m water system membrane filtration is to be measured in sample injection bottle.
2) mensuration of honey protein hydrolytic amino acid: amino-acid analyzer adopts gradient elution, and the sample determination time is 53min, separates 57 DEG C of column temperatures, reaction column column temperature 135, damping fluid flow velocity 0.4mL/min, triketohydrindene hydrate flow velocity 0.35mL/min.Passage 1: detect wavelength 570nm, passage 2: detect wavelength 440nm, sample size 20 μ L, with the each amino acid whose content of external standard method calculating.
3) data processing: PLS-DA is realized by the tool box PLS Toolbox3.5 of MATLAB 7.1.PLS-DA is made as class variable by Y variable in analyzing, and carries out linear regression by the Argine Monohydrochloride spectrum of class variable and honey sample, differentiates for two classes, and the Y variate-value of chaste honey and rape honey is set as respectively 0 and 1, and Threshold is 0.5.Concrete criterion is: as deviation < 0.5, judge that sample belongs to such; As deviation > 0.5, judge that sample does not belong to such; When deviation=0.5, judge that sample classification is indefinite.Because Cys and Met are in acid hydrolysis process, easily degraded, causes measured value error larger, for ensureing the accuracy of result, does not participate in the foundation of model.
In 56 samples measuring, software extracts 39 samples randomly as calibration set, for the validation-cross of model foundation and model; Remaining 17 samples, as checking collection, for testing model, do not participate in modeling.In honey sample, protein hydrolytic amino acid has been measured 17 kinds altogether, in table 1.
Table 1 twigs of the chaste tree and rape honey protein hydrolytic amino acid
4) foundation of PLS-DA discrimination model and checking: adopt PLS-DA techniques of discriminant analysis that the amino acid content in the honey sample recording and classified variable are carried out to linear regression, to 39 of calibration set honey Sample Establishing discrimination models, Fig. 1 has provided the relation between chaste honey and PLS predicted value and the measured value of rape honey sample classification variable in calibration set, the sample of predicted value between 0 ± 0.5 is chaste honey sample, and predicted value is rape honey between 1 ± 0.5.As can be seen from Table 2, discrimination model is to 2 chaste honeys and 1 rape honey erroneous judgement, and always differentiation rate is 92.3%.
Correction and the result of table 2 PLS-DA model
The calibration model that utilizes PLS-DA method to set up, carries out check analysis to 17 samples that have neither part nor lot in modeling, from Fig. 2 and table 2, can find out, only a chaste honey is judged by accident, always differentiation rate is 94.1%.
Claims (6)
1. a discrimination method for rape honey and chaste honey, is characterized in that, comprises the following steps:
(1) build and differentiate model:
Sample to the rape honey providing in advance and chaste honey is processed, and measures honey protein hydrolytic amino acid, and the sample number of every kind of honey is no less than 15;
Y variable is made as to classified variable, and the Y variate-value of chaste honey and rape honey is set as respectively 0 and 1, and Threshold is 0.5, adopts partial least squares discriminant analysis method that the amino acid content in the sample recording and classified variable are carried out to linear regression, sets up and differentiates model;
(2) differentiate:
Honey to be identified is processed, measured honey protein hydrolytic amino acid, according to the amino acid content recording, the discriminating model that utilizes step (1) to obtain is differentiated, determines that honey to be identified belongs to chaste honey or rape honey.
2. the discrimination method of rape honey according to claim 1 and chaste honey, is characterized in that, the assay method of honey protein hydrolytic amino acid comprises the following steps:
1. the water that adds 2～3 times of volumes in honey, mixes, and gets supernatant after centrifugal treating;
2. adopt the 1. middle supernatant obtaining of trichloroacetic acid freezing treatment step, obtain honey albumen precipitation;
3. honey albumen precipitation is transferred in hydrolysis pipe to acid hydrolysis honey albumen under vacuum condition with hydrochloric acid solution;
4. adopt automatic amino acid analyser to measure honey protein hydrolytic amino acid.
3. the discrimination method of rape honey according to claim 2 and chaste honey, is characterized in that:
Step 1. in, centrifugal treating is at 1500g, under 4 DEG C of conditions, centrifugal 10min.
4. the discrimination method of rape honey according to claim 2 and chaste honey, is characterized in that:
Step 2. in, trichloroacetic acid freezing is specially, in supernatant, add 50%～100% the trichloroacetic acid that is equivalent to honey volume, fully mix, after-20 DEG C of placement 15min, then place 1h in 4 DEG C, make the albumen precipitation in honey, by centrifuge tube in 4 DEG C, centrifugal 10min under 10000g condition, abandoning supernatant.
5. the discrimination method of rape honey according to claim 2 and chaste honey, is characterized in that:
Step concrete grammar is 3., the hydrochloric acid solution of employing 6.0mol/L divides to be transferred to albumen precipitation in hydrolysis pipe for three times completely, be filled with after nitrogen, be evacuated to vacuum with vacuum pump, will hydrolysis channel closure and be hydrolyzed 24h in the thermostatic drying chamber of 110 DEG C, take out to be cooled to room temperature, by the common Filter paper filtering of hydrolyzate, filtrate nitrogen at 50 DEG C dries up, and finally residue is used to 0.02mol/L dissolve with hydrochloric acid solution, 0.25 μ m water system membrane filtration, obtains testing sample.
6. the discrimination method of rape honey according to claim 2 and chaste honey, it is characterized in that: at least measure following 15 seed amino acid content, Asp, Thr, Ser, Glu, Gly, Ala, Val, Ile, Leu, Tyr, Phe, Lys, His, Arg, Pro.
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| CN104849232B (en) * | 2015-04-27 | 2019-02-01 | 中国农业科学院蜜蜂研究所 | A kind of method of quick detection royal jelly moisture and protein content |
| CN105044230A (en) * | 2015-06-30 | 2015-11-11 | 西北大学 | Method for identifying linden honey, vicia villosa Roth honey and rape honey |
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| CN107515256A (en) * | 2017-05-08 | 2017-12-26 | 西北大学 | A kind of method for differentiating Mel Jujubae, chaste honey, acacia honey and honey of lungan flowers |
| CN108152413A (en) * | 2017-12-21 | 2018-06-12 | 西北大学 | A kind of chaste honey discrimination method based on amino acid |
| CN111458422B (en) * | 2020-03-13 | 2022-06-17 | 中国农业科学院蜜蜂研究所 | Identification method of mature rape honey |
| CN111458421B (en) * | 2020-03-13 | 2022-06-17 | 中国农业科学院蜜蜂研究所 | Identification method of mature rape honey |
| CN111426776B (en) * | 2020-06-12 | 2020-10-23 | 中国农业科学院蜜蜂研究所 | Application of HQR as characteristic marker of schefflera octophylla honey |
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