CN107561110A - A kind of discrimination method for being used for chaste honey, rape honey and acacia honey based on nuclear magnetic resonance technique - Google Patents
A kind of discrimination method for being used for chaste honey, rape honey and acacia honey based on nuclear magnetic resonance technique Download PDFInfo
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- 238000000034 method Methods 0.000 title claims abstract description 29
- 238000005481 NMR spectroscopy Methods 0.000 title claims abstract description 24
- 238000012850 discrimination method Methods 0.000 title claims abstract description 7
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- 239000011734 sodium Substances 0.000 claims description 7
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- 125000000217 alkyl group Chemical group 0.000 claims 1
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- MQVMJSWYKLYFIG-UHFFFAOYSA-N propane-1-sulfonic acid;sodium Chemical compound [Na].CCCS(O)(=O)=O MQVMJSWYKLYFIG-UHFFFAOYSA-N 0.000 abstract 1
- 125000000026 trimethylsilyl group Chemical group [H]C([H])([H])[Si]([*])(C([H])([H])[H])C([H])([H])[H] 0.000 abstract 1
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Abstract
The invention discloses a kind of discrimination method for being used for chaste honey, rape honey and acacia honey based on nuclear magnetic resonance technique, by honey sample, is configured to 0.03 0.5g/L solution after filtering with heavy water；Add the phosphate buffer solution that concentration is 0.5 2.0 mol/L, wherein, containing the propyl sulfonic acid sodium inner mark solution of 3 trimethylsilyl 1 that volume fraction is 0.05 0.3% and 0.1 3.0 mM sodium azide in phosphate buffer solution, mixing, it is 2.5 4.0 to adjust pH, determines to obtain nuclear magnetic resoance spectrum through nuclear magnetic resonance spectrometer；Honey sample label chemical shift is analyzed,1The deviation △ δ that H chemical shifts δ is 7.0ppm~7.5ppm are chaste honey within 0.02 0.05ppm scopes, are otherwise rape honey or acacia honey.This method a large amount of samples of analysis, quick discriminating can go out to divide chaste honey and rape honey and acacia honey in the short time.
Description
Technical field
The present invention relates to being originally related to belong to food inspection, it is more particularly to one kind and the twigs of the chaste tree is used for based on nuclear magnetic resonance technique
The discrimination method of honey, rape honey and acacia honey.
Background technology
Provided in honey standard GB/T 14963-2011GB, honey is a kind of nectar, secretion of honeybee herborization
Or honeydew, the natural sweet substance through fully brewageing, it is a kind of nutritious natural taste after being mixed with itself secretion
Support food.Hua Yuan is variant, i.e. the metabolism of plant is variant, thus the nectar compositions that honeybee is adopted will be different, and honey is usual
Classified according to nectariferous plant, rape honey, acacia honey, chaste honey, Mel Jujubae, Mel etc. can be divided into.In recent years, it is domestic and
International market constantly expands to the demand of honey, but the yield of honey is but difficult to meet the market demand.Due to China region
It is vast, with a varied topography, weather is various, honey honey kind and the place of production there is diversified characteristic, its added value of product also produces difference.
Under the driving of tremendous economic interests, many criminals are added other low-quality honey in high-quality honey and filled with secondary
It is good, reach the effect mixed the spurious with the genuine.The severe jamming market order of honey product and the export trade of China's honey product.Cause
This needs to develop effective, reliable method to differentiate the honey of different plant sources.
Discriminating for honey honey kind, maximally effective means are the spirits for finding significantly to distinguish specific honey kind parameter
Quick, reliable chemical marker.Conventional method differentiates mainly by sense organ and pollen analysis.Sense organ differentiate be by seeing, hearing, product,
It was found that variety classes honey some existing differences in terms of color and luster, smell, mouthfeel, and then distinguish and differentiate.This method has very big
Limitation, depend on the personal experience of testing staff；Pollen analysis is to observe pollen cell in honey under the microscope
Form, because the pollen of every kind of nectariferous plant has the feature of oneself, therefore the honey kind of honey can be differentiated.But the honeybee of some honey kinds
Bee pollen is similar, and this method is difficult to distinguish.However, the international standard about special sign thing is not promulgated also.European Council is sent out
Cloth determination honey honey kind mirror method for distinguishing, includes determining general flavone, volatile component, amino acid, metal and nonmetallic trace
Secondary element.But these methods lack sensitive reliable mark, the discriminating for honey honey kind, its accuracy, sensitivity and
Reliability will all substantially reduce.
Nuclear magnetic resonance (NMR) is a kind of very important research and analysis testing tool, in chemistry, biology, medical science etc.
It is used widely in field, there are many advantages：The integrality of test object can be kept, does not destroy the property of sample；To sample
This requirement is not harsh, can quickly handle, and repeats to test, greatly reduces the consumption of experiment；The discriminating to material can be completed simultaneously
It is efficiently quick with the measure of content of material；With fabulous resolution ratio.The present invention filters out chaste honey with nuclear magnetic resonance technique
Characteristic indication thing, so as to establish the quick method for distinguishing chaste honey, rape honey and acacia honey.
The content of the invention
The invention provides：A kind of discrimination method for being used for chaste honey, rape honey and acacia honey based on nuclear magnetic resonance technique,
Technically reliable, a large amount of samples of analysis, quick discriminating it can go out to divide chaste honey and rape honey and acacia honey in the short time, avoid subjectivity
The influence of factor, human error, accuracy is high, conclusion science is reliable.
In order to solve the above problems, the technical solution adopted in the present invention is such, and one kind is based on nuclear magnetic resonance technique
For the discrimination method of chaste honey, rape honey and acacia honey, comprise the following steps,
1）The honey sample that will be stirred, filter-cloth filtering, remove in honey after solid impurity, 0.03- is configured to heavy water
0.5g/L solution；Described honey sample is chaste honey, rape honey and acacia honey；
2）The above-mentioned solution of certain volume is taken, adds the phosphate buffer solution that concentration is 0.5-2.0 mol/L, both volumes
Than for 800-1500：100-300, wherein, containing the 3- trimethyl silanes that volume fraction is 0.05-0.3% in phosphate buffer solution
The sodium azide of base -1- propyl sulfonic acid sodium inner mark solutions and 0.1-3.0 mM, vortex oscillation adjust final solution to uniform mixing
PH value be 2.5-4.0, be placed in nuclear magnetic tube；
3）Nuclear magnetic tube is positioned in nuclear magnetic resonance spectrometer, detection obtains nuclear magnetic resoance spectrum；The analysis condition of NMR spectrum
For：Popped one's head in using BBI；Measurement temperature:20-35 DEG C of room temperature；Ambient humidity: 20-35%;The MHz of observed frequency 400；Using
Presaturation method suppresses water peak；Pulse protocol is：Noesygppr1d either zg30 or zgpr；Spectrum width: 6410 Hz；90 ° of arteries and veins
Rush width: pl= 6. 45μs;Pulse delay time: dl= 15 s；Launching centre: O1=4.7；Accumulative frequency:16 or
64；
4）Honey sample label chemical shift is analyzed,1H chemical shifts δ is 7.0ppm~7.5ppm ± 0.02-0.05ppm
Have within scope multiplet for chaste honey, be otherwise rape honey or acacia honey.
Above-mentioned honey sample is divided into nodeless mesh and crystallization, to the honey sample of nodeless mesh, is stirred before filtering
；To there is the honey sample of crystallization, in the case of closed, it be placed in the water-bath no more than 40 DEG C -60 DEG C and warm, vibrates, treat
Sample stirs evenly after all melting, and is rapidly cooled to room temperature；
Preferably, honey sample filtering uses nylon filtering cloth of the aperture for 0.10mm-0.14mm.
Preferably step 2）Concentration is 1.0 mol/L hydrochloric acid or Strong oxdiative sodium used by adjusting the pH value of final solution.
In order to ensure the accuracy of looked for label, we have investigated the situation of the honey sample of different sources, honey sample
Product provenance is in Jiangsu, Henan, Xinjiang, Sichuan, Inner Mongol, Hubei, Liaoning, Jilin, Shaanxi or Shandong.
By the nmr spectrum of the chaste honey of comparative studies different sources, find all chaste honeys in this chemical shift
Go out and higher corresponding multiplet all be present, meanwhile, existed by comparative studies different sources rape honey and acacia honey1H chemical shifts
Whether δ has interference for 7.0ppm~7.5ppm's, the results showed that all rape honeys and acacia honey are all noiseless herein.Therefore
It is final to determine1The multiplet that H chemical shifts δ is 7.0ppm~7.5ppm is the distinctive characteristic indication thing of chaste honey, Ke Yizuo
To distinguish chaste honey and rape honey and the feature difference material of acacia honey.
Beneficial effect：The technology of the present invention is reliable, and a large amount of samples can be analyzed in the short time, and quick discriminating goes out to divide chaste honey and oil
Dish honey and acacia honey, the influence of subjective factor, human error is avoided, accuracy is high, conclusion science is reliable.
Brief description of the drawings
Fig. 1 is the nuclear magnetic spectrogram of Henan chaste honey；
Fig. 2 is the nuclear magnetic spectrogram of Henan rape honey；
Fig. 3 is the nuclear magnetic spectrogram of Henan acacia honey.
Embodiment
By detailed description below to further explanation of the present invention, and line justification is entered to advantage of the present invention.
Experimental facilities includes：The type NMRs of Advance 400（Brooker,Switzerland company）, 14.1 T superconducting magnets,
5 mm double-core z- gradient probes and the controlling tests of Topspin 2.3 and data processing software；5mm nuclear magnetic resonance sample pipes；At a high speed
Centrifuge（Sigma, German company）；Turbine mixer（XW-80A types, Instrument Factory, Shanghai Medical Science Univ.）；LP403 assay balances
（Sai Duolisi, German company）；
Test solvent includes：Deuterated water（Deuterium band width is 99.8%, also known as heavy water）It is purchased from Cambrideg Isotope
Laboratories companies；3- trimethylsilyl -1- propyl sulfonic acid sodium（TSPSA）It is purchased from Aldich-Sigma companies；Phosphoric acid
Hydrogen dipotassium and sodium dihydrogen phosphate（Top pure grade）It is purchased from Aldich-Sigma companies.
1st, the confirmation of chaste honey mark
The collection of 1.1 honey samples
Voluntarily collection honey sample, which amounts to 60, includes chaste honey 20, rape honey 20 and acacia honey 20；The place of production being related to
Including：Jiangsu, Henan, Xinjiang, Sichuan, Inner Mongol, Hubei, Liaoning, Jilin, Shaanxi, Shandong；
1.2. the pre-treatment of honey sample
To nodeless mesh in honey sample, it is stirred for before filtering uniformly；And to there is crystallization, in the case of closed, put
Warm, vibrate in the water-bath no more than 60 DEG C, stirred evenly after sample all melts, be rapidly cooled to room temperature；Through above-mentioned processing
Known honey sample afterwards, filtered through 0.10mm-0.14mm apertures nylon filtering cloth, remove solid impurity in honey, take 0.1 g samples
Product add 1 mL heavy water in centrifuge tube, and dissolving is complete；
The above-mentioned μ l of solution 800 are taken, add the phosphate buffer solution that 100 μ l concentration are 0.5 mol/L（pH=2.0）, wherein buffering
Containing the 3- trimethylsilyl -1- propyl sulfonic acid sodium inner mark solutions that volume fraction is 0.05% and 0.1 mM Azide in solution
Sodium, vortex oscillation is to uniform mixing, and then with 1.0 mol/L hydrochloric acid or Strong oxdiative sodium, the pH value for adjusting final solution is
2.5, wherein 600 μ l are taken in nuclear magnetic tube.
1.3. the foundation of nmr analysis
Adjust magnetic resonance spectroscopy instrument and nuclear magnetic tube is positioned in nuclear magnetic resonance chemical analyser, rotation nuclear magnetic tube obtains in case NMR detections
To the nuclear magnetic signal of honey sample；The analysis condition of NMR spectrum is：Popped one's head in using BBI；Measurement temperature（Probe temperature）:
20-35 DEG C of room temperature；Ambient humidity: 20-35%;The MHz of observed frequency 400；Water peak is suppressed using presaturation method；Pulse journey
Sequence is：Noesygppr1d either zg30 or zgpr；Spectrum width: 6410 Hz；90 ° of pulse widths: pl= 6. 45μs;Arteries and veins
Rush time delay: dl= 15 s；Launching centre: O1=4.7；Accumulative frequency:16 or 64.
1.4. spectrogram pre-processes
Carrying out Fourier to the NMR signal of gained with the data processing software that nuclear magnetic resonance spectrometer carries becomes to change, conversion
Count as 131072, index linewidth factor is 1Hz, obtains the nuclear magnetic spectrum of sample.
With topspin softwares（Each parameter setting is as follows in Topspin softwares：PULPROG= Jresgpprqf, AQ_mod
=DQD, TD=32K, NS=8*N, DS=4, the μ of TD0=1, SW=6000 Hz, D1=3 s, DE=4 s, D8=0.1s, signal
It is cumulative 16 times））The original fingerprint collection of illustrative plates of acquisition is pre-processed, including spectral peak alignment, baseline correction and phasing.With 3-
Trimethylsilyl -1- propyl sulfonic acid sodium does internal standard compound, and chemical shift is set to 0.00 carry out spectral peak alignment；Baseline correction selects
Polynomial fit fit approach；Mutually correction selection global and metabonomics algorithms elder generation Automatic Optimal, it is rear for spy
Determine region carry out manual correction, make integrated value as much as possible be on the occasion of.
1.5. the comparison of nmr spectrum
By the nmr spectrum of comparative studies chaste honey, rape honey and acacia honey, it is found that chaste honey exists1H chemical shifts δ
The higher multiplet of response between 7.0ppm~7.5ppm be present.
By the nmr spectrum of the chaste honey of comparative studies different sources, find all chaste honeys in this chemical shift
Go out and higher corresponding multiplet all be present,
Meanwhile existed by comparative studies different sources rape honey and acacia honey1H chemical shifts δ is 7.0ppm~7.5ppm
Whether have interference, the results showed that all rape honeys and acacia honey are all noiseless herein.
Therefore, it is final to determine1The multiplet that H chemical shifts δ is 7.0ppm~7.5ppm is the distinctive feature of chaste honey
Mark, can be as the feature difference material for distinguishing chaste honey and rape honey and acacia honey.Such as the core that Fig. 1 is Henan chaste honey
Magnetic spectrum figure；Fig. 2 is the nuclear magnetic spectrogram of Henan rape honey；Fig. 3 is the nuclear magnetic spectrogram of Henan acacia honey.
2nd, the detection of actual sample
It is used to examine unknown honey sample with the method for quick identification of the discriminating chaste honey, rape honey and acacia honey of foundation
Survey.20 parts of unknown honey samples are operated by the method for above-mentioned steps 1,2 ~ 1.4, obtain the nuclear magnetic resonance of all samples
Spectrogram, the label according to the chaste honey found in step 5 are judged unknown sample.Detected under identical experiment condition
Sample and chaste honey mark1H chemical shifts δ is 7.0ppm~7.5ppm deviation △ δ in 0.02-0.05ppm scopes
Within, then it is assumed that it is chaste honey, is otherwise rape honey or acacia honey, quickly can be distinguished according to this from rape honey and acacia honey
Do not go out chaste honey, concrete outcome is as shown in table 1, and 10 chaste honeys are obtained for good identification in 20 samples, differentiates correct
Rate is 100%.
Table 1
| Sample type | Legitimate reading | Detect result |
| Chaste honey（10） | The twigs of the chaste tree | The twigs of the chaste tree |
| Rape honey and acacia honey（10） | Rape or acacia | Rape or acacia |
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, it is all the present invention spirit and
Within principle, any modification, equivalent substitution and improvements made etc., it should be included in the scope of the protection.
Claims (5)
- A kind of 1. discrimination method for being used for chaste honey, rape honey and acacia honey based on nuclear magnetic resonance technique, it is characterised in that including Following steps,1）The honey sample that will be stirred, filter-cloth filtering, remove in honey after solid impurity, 0.03- is configured to heavy water 0.5g/L solution；Described honey sample is chaste honey, rape honey and acacia honey；2）The above-mentioned solution of certain volume is taken, adds the phosphate buffer solution that concentration is 0.5-2.0 mol/L, both volumes Than for 800-1500：100-300, wherein, containing the 3- trimethyl silicanes that volume fraction is 0.05-0.3% in phosphate buffer solution The sodium azide of alkyl -1- propyl sulfonic acid sodium inner mark solutions and 0.1-3.0 mM, vortex oscillation to uniform mixing, adjustment are final molten The pH value of liquid is 2.5-4.0, is placed in nuclear magnetic tube；3）Nuclear magnetic tube is positioned in nuclear magnetic resonance spectrometer, detection obtains nuclear magnetic resoance spectrum；The analysis condition of NMR spectrum For：Popped one's head in using BBI；Measurement temperature:20-35 DEG C of room temperature；Ambient humidity: 20-35%;The MHz of observed frequency 400；Using Presaturation method suppresses water peak；Pulse protocol is：Noesygppr1d either zg30 or zgpr；Spectrum width: 6410 Hz；90 ° of arteries and veins Rush width: pl= 6. 45μs;Pulse delay time: dl= 15 s；Launching centre: O1=4.7；Accumulative frequency:16 or 64；4）Honey sample label chemical shift is analyzed,1H chemical shifts δ is 7.0ppm~7.5ppm ± 0.02-0.05ppm Have within scope multiplet for chaste honey, be otherwise rape honey or acacia honey.
- A kind of 2. discriminating for being used for chaste honey, rape honey and acacia honey based on nuclear magnetic resonance technique according to claim 1 Method, it is characterised in that for the honey sample of crystallization, before stirring, in the case of closed, be placed in no more than 40-60 DEG C Water-bath in warm, vibrate, treat sample all melt, after stirring, then be rapidly cooled to room temperature.
- A kind of 3. discriminating for being used for chaste honey, rape honey and acacia honey based on nuclear magnetic resonance technique according to claim 1 Method, it is characterised in that honey sample filtering uses nylon filtering cloth of the aperture for 0.10mm-0.14mm.
- A kind of 4. discriminating for being used for chaste honey, rape honey and acacia honey based on nuclear magnetic resonance technique according to claim 1 Method, it is characterised in that step 2）Concentration is 1.0 mol/L hydrochloric acid or Strong oxdiative used by adjusting the pH value of final solution Sodium.
- 5. a kind of according to claim 1 is used for chaste honey, rape honey and rape acacia honey based on nuclear magnetic resonance technique Discrimination method, it is characterised in that honey sample provenance is in Jiangsu, Henan, Xinjiang, Sichuan, Inner Mongol, Hubei, Liaoning, Ji Woods, Shaanxi or Shandong.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108614000A (en) * | 2018-04-13 | 2018-10-02 | 江苏出入境检验检疫局动植物与食品检测中心 | Manuka honey discrimination method based on SIMCA models |
| CN108872289A (en) * | 2018-04-13 | 2018-11-23 | 江苏出入境检验检疫局动植物与食品检测中心 | Manuka honey discrimination method based on nuclear magnetic resonance technique |
| CN109444200A (en) * | 2018-12-21 | 2019-03-08 | 江苏中谱检测有限公司 | A method of northeast eucalyptus honey is identified using nuclear magnetic resonance spectroscopy finger-print |
| CN111380895A (en) * | 2020-04-01 | 2020-07-07 | 江苏中谱检测有限公司 | Nuclear magnetic resonance hydrogen spectrometry for identifying whey protein powder added in formula powder |
| CN111380896A (en) * | 2020-04-07 | 2020-07-07 | 江苏中谱检测有限公司 | Method for identifying mature and concentrated rape honey, locust honey and chaste tree honey by using pyruvic acid |
| EA037558B1 (en) * | 2019-01-22 | 2021-04-14 | Федеральное государственное автономное образовательное учреждение высшего образования "Северо-Восточный федеральный университет имени М.К. Аммосова" | Method for determining the impact of high temperatures on honey |
| CN113933334A (en) * | 2021-10-13 | 2022-01-14 | 北京工商大学 | Feature selection and machine learning algorithm-based acacia honey authenticity identification method |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20070055456A1 (en) * | 2005-08-31 | 2007-03-08 | Daniel Raftery | NMR method for differentiating complex mixtures |
| CN104713895A (en) * | 2015-03-13 | 2015-06-17 | 中国科学院武汉物理与数学研究所 | Method for distinguishing between pure and syrup-adulterated honey based on combination of hydrogen nuclear magnetic resonance and partial least square method |
| CN105510372A (en) * | 2016-01-27 | 2016-04-20 | 江苏出入境检验检疫局动植物与食品检测中心 | Method for building model for DPLS-BS-UVE rapid honey identification |
| CN105548233A (en) * | 2015-10-30 | 2016-05-04 | 中国科学院武汉物理与数学研究所 | Method for discriminating acacia honey and rape honey on basis of H-nuclear magnetic resonance |
-
2017
- 2017-08-25 CN CN201710742918.7A patent/CN107561110B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20070055456A1 (en) * | 2005-08-31 | 2007-03-08 | Daniel Raftery | NMR method for differentiating complex mixtures |
| CN104713895A (en) * | 2015-03-13 | 2015-06-17 | 中国科学院武汉物理与数学研究所 | Method for distinguishing between pure and syrup-adulterated honey based on combination of hydrogen nuclear magnetic resonance and partial least square method |
| CN105548233A (en) * | 2015-10-30 | 2016-05-04 | 中国科学院武汉物理与数学研究所 | Method for discriminating acacia honey and rape honey on basis of H-nuclear magnetic resonance |
| CN105510372A (en) * | 2016-01-27 | 2016-04-20 | 江苏出入境检验检疫局动植物与食品检测中心 | Method for building model for DPLS-BS-UVE rapid honey identification |
Non-Patent Citations (1)
| Title |
|---|
| XIN ZHENG ET AL.: "Origin Identification and Quantitative Analysis of Honeys by Nuclear Magnetic Resonance and Chemometric Techniques", 《FOOD ANAL. METHODS》 * |
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108614000A (en) * | 2018-04-13 | 2018-10-02 | 江苏出入境检验检疫局动植物与食品检测中心 | Manuka honey discrimination method based on SIMCA models |
| CN108872289A (en) * | 2018-04-13 | 2018-11-23 | 江苏出入境检验检疫局动植物与食品检测中心 | Manuka honey discrimination method based on nuclear magnetic resonance technique |
| CN109444200A (en) * | 2018-12-21 | 2019-03-08 | 江苏中谱检测有限公司 | A method of northeast eucalyptus honey is identified using nuclear magnetic resonance spectroscopy finger-print |
| EA037558B1 (en) * | 2019-01-22 | 2021-04-14 | Федеральное государственное автономное образовательное учреждение высшего образования "Северо-Восточный федеральный университет имени М.К. Аммосова" | Method for determining the impact of high temperatures on honey |
| CN111380895A (en) * | 2020-04-01 | 2020-07-07 | 江苏中谱检测有限公司 | Nuclear magnetic resonance hydrogen spectrometry for identifying whey protein powder added in formula powder |
| CN111380896A (en) * | 2020-04-07 | 2020-07-07 | 江苏中谱检测有限公司 | Method for identifying mature and concentrated rape honey, locust honey and chaste tree honey by using pyruvic acid |
| CN113933334A (en) * | 2021-10-13 | 2022-01-14 | 北京工商大学 | Feature selection and machine learning algorithm-based acacia honey authenticity identification method |
| CN113933334B (en) * | 2021-10-13 | 2024-03-26 | 北京工商大学 | Locust honey authenticity identification method based on feature selection and machine learning algorithm |
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