CN108872289A - Manuka honey discrimination method based on nuclear magnetic resonance technique - Google Patents
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Abstract
The invention belongs to field of food safety, especially Manuka honey identifies field, more particularly relate to the Manuka honey discrimination method based on nuclear magnetic resonance technique, this method determines whether sample to be tested is Manuka honey by the NMR spectrum spectral data of analysis sample to be tested.Manuka honey discrimination method disclosed by the invention based on nuclear magnetic resonance can make up defect present in adulterated Manuka honey identification at present by specific characteristic indication object.This method has many advantages, such as that analysis time is short, integrality is strong, specificity is good, controllability is strong, accuracy is high.It the use of after discrimination method disclosed in this invention is 10% for the limit of identification of Mai Luka characteristic indication object ingredient contained in Manuka honey.
Description
Technical field
The invention belongs to field of food safety, especially Manuka honeys to identify field, more particularly relate to base
In the Manuka honey discrimination method of nuclear magnetic resonance technique.
Background technique
Mai Luka (Manuka) honey is a kind of distinctive precious honey kind of New Zealand, is honeybee acquisition New Zealand distinctive one
Kind shrub plant --- Manuka (Leptospermum scoparium) nectar brewing made of.Since Manuka honey has
There is unique antibacterial activity, can be used for preventing wound infection, helps wound healing, medical value with higher, therefore it is more next
Favor more by China consumer.
Currently, Zelanian Manuka honey outlet is annual in the past 10 years to increase by 10% or so, 2013, go out from New Zealand
The honey of mouth is worth 1.28 hundred million New Zealand Dollars.According to the statistics of one beekeeper association of New Zealand, New Zealand only about produces every year
1700-2000 tons of Manuka honey, and in the world, every year with the honey that Mai Luka name is sold be up to 10,000 tons with
On.Similarly, specific gravity shared by Manuka honey of the import to China is also increasing year by year.
On the one hand, there are a small number of illegal businessman in order to seek exorbitant profit, mixed in pure Manuka honey relatively cheap
Syrup, this causes very big negative effect to inlet and outlet bee's product market, has cheated the majority of consumers, other than syrup is adulterated,
The honey of other types is also frequently present of for Manuka honey to be adulterated, and the latter is often more difficult to identify.On the other hand, due to
Manuka honey is to carry out quality evaluation and classification, the Manuka honey price difference of different stage according to its antibacterial activity height
It is different huge.Artificial synthesized methyl-glyoxal is illegally added in Manuka honey（methylglyoxal, MGO）Or dihydroxyacetone (DHA)
（DHA）It is reaped staggering profits with improving activity.
The discrimination method of Mai Luka is mainly issued by Manuka honey relevant government department of New Zealand, and propionic aldehyde ketone is commonly used
（MGO）Or dihydroxyacetone (DHA)（DHA）The rank of Content evaluation Mai Luka honey, but both can be artificial adulterated.New Zealand Mai Luka
Association（UMFHA）It was found that the characteristic compounds and its content and anti-of leoptosperin and NSC 611398 as Manuka honey
Bacterium activity is related.Official of New Zealand is a kind of based on science, accurate and reliable Manuka honey standard of perfection in order to establish, at the beginning of New Zealand
Grade Estate Division（Ministry for Primary Industries, MPI）By 3 years scientific planning items, in April, 2017
It discloses while can distinguish single flower kind Mai Luka honey, spend more kind of Mai Luka honey and a non-Manuka honey standard of perfection, it is final true
Determine 2'- methoxyacetophenone（2'-MAP）, O-Anisic Acid（2-MBA）, 3-phenyl lactic acid（3-PA）With 4- hydroxy phenyl
Lactic acid（4-HPA）These four compounds can be used as the index for determining Manuka honey.But Manuka honey criterion lacks
Unified, leading to honey market, the good and bad jumbled together.
China has put into effect the mandatory national standards GB 14963-2011 about honey in 2011, mainly from moisture, fruit
Sugar and three compulsory indexes of glucose total amount and cane sugar content judge that the quality of honey, the standard can be used for judging Mai Luka
The quality of honey.But since the detection parameters of new national standard are relatively easy, it is difficult effectively to identify the adulterated of Manuka honey.For
The method that the doping of new national standard is faked continuously emerges, and Manuka honey its indices after doping can meet wanting for national standard
It asks.Meanwhile the country is substantially at blank for the research of Manuka honey at present, this supervises the supervision of import Manuka honey
Pipe, and ensure that the legitimate rights and interests of China consumer can all make a big impact.Therefore, effective, sensitive honey adulteration is developed
Detection method becomes extremely urgent, is badly in need of domestic progress correlative study and formulates standard to be supervised.
Nmr analysis is the structure and property that substance is analyzed by the measurement of Nmr Lines characteristic parameter
Matter, it can not destroy the internal structure of sample, be a kind of completely lossless detection method.Meanwhile magnetic resonance detection
Analysis method has very high resolving power and accuracy, and sample pretreatment is simple, is therefore widely used in physics, changes
, medical treatment, petrochemical industry, archaeology etc..
Summary of the invention
Goal of the invention of the invention is to provide a kind of Manuka honey discrimination method based on nuclear magnetic resonance.
In order to realize this goal of the invention, the invention discloses the Manuka honey identification sides based on nuclear magnetic resonance technique
Method, this method determine whether sample to be tested is Mai Luka by the NMR spectrum spectral data of analysis sample to be tested
Honey is specifically described as：
A. when spectral analysis of the nuclear magnetic resonance map meets the following conditions simultaneously, which is Manuka honey：
（1）Contain1H chemical shift δ be 2.30 ± 0.05ppm, two of 2.38 ± 0.05ppm it is unimodal；
（2）Unimodal height is higher than unimodal height at 2.38ppm at 2.30ppm, and two unimodal relative height ratios are more than or equal to
2.0；
（3）The error range of spectral peak height is no more than 10%；
B. when spectral analysis of the nuclear magnetic resonance map be unsatisfactory for it is above（1）-（3）When middle either condition, which is not wheat
Lu's card honey.
Wherein1H chemical shift δ is 2.30 ± 0.05ppm, two of 2.38 ± 0.05ppm it is unimodal for institute of the invention really
The vertical characteristic indication object to identify Manuka honey.This feature marker be different from the prior art commonly used by 2'- first
Oxygroup acetophenone（2'-MAP）, O-Anisic Acid（2-MBA）, 3-phenyl lactic acid（3-PA）With 4- hydroxy phenyl lactic acid（4-
HPA）Four kinds of monomer indexs.Two unimodal representative ingredients as characteristic indication object are not a certain monomeric compounds, and
It is with the mixture of more abundant index parameter, the two are unimodal by 114 ceromel samples（Including Manuka honey,
Block slave's card honey, Rui Waruiwa honey, Ka Maxi honey, Christmas flower honey, auspicious tower honey, Tahoua 7 kinds of auspicious honey）With 50
A commercialization Manuka honey sample analysis obtains, and is the characteristic indication object that can stablize mark Manuka honey.Unimodal goes out
Peak retention time and opposite peak height can accurately distinguish Manuka honey, and its unimodal interior information content is high, more existing monomer
For index, artificial addition monomeric compound false making can be effectively prevented.
The analysis condition that the present invention further discloses NMR spectrum is：It is popped one's head in using BBI；Measuring temperature：Room temperature
20-35 ℃；Ambient humidity： 20-35%；400 MHz of observed frequency；Water peak is suppressed using presaturation method；Pulse protocol is：
Noesygppr1d is zg30 or is zgpr；Spectrum width：6410 Hz；90 ° of pulse widths： pl= 6. 45μs；Pulse is prolonged
The slow time： dl= 15 s；Launching centre： O1=4.7；Accumulative frequency：16 or be 64.
Further, the present invention discloses spectral analysis of the nuclear magnetic resonance sample preparation methods and is：Into honey sample solution,
The phosphate buffer solution that concentration is 0.5-2.0 mol/L is added, the volume ratio of the two is 800-1500：100-300 is vortexed
Oscillation adjusts the pH value of solution to 2.5-4.0 to uniform mixing, take wherein 600 μ l in nuclear magnetic tube.
The solution for adjusting the pH value of solution preferably wherein is hydrochloric acid or sodium hydroxide.
More preferably, the concentration of the hydrochloric acid or sodium hydroxide is 1.0mol/L.
Wherein, the 3- trimethylsilyl -1- propyl sulfonic acid for being 0.05-0.3% containing volume fraction in phosphate buffer solution
The sodium azide of sodium inner mark solution and 0.1-3.0 mM.
It is further preferable that the preparation method that the present invention further discloses honey sample solution is：By the honey sample after thawing
Product are filtered through nylon filtering cloth, in removing honey after solid impurity, accurately weigh 0.25 g sample in centrifuge tube, 1mL is added
Heavy water, dissolution are complete.
Preferably, the aperture of the nylon filtering cloth is 0.10mm-0.14mm.
It still further preferably discloses in the present invention and is by the thawing processing step of honey sample：To the laboratory of nodeless mesh
Sample is stirred for uniformly, to the sample for having crystallization, in closed situation, being placed in the water-bath no more than 60 DEG C and warming, shake
It swings, is stirred evenly after sample all melts, be rapidly cooled to room temperature.
Manuka honey discrimination method disclosed by the invention based on nuclear magnetic resonance, can be with by specific characteristic indication object
Make up defect present in adulterated Manuka honey identification at present.This method is short with analysis time, integrality is strong, specificity
Well, the advantages that controllability is strong, accuracy is high.Using after discrimination method disclosed in this invention for contained in Manuka honey
Mai Luka characteristic indication object ingredient limit of identification be 10%.
Popularization and implementation of the invention can preferably establish China laboratory in Manuka honey detection technique field
Right of speech, to cope with or providing technical support for counter foreign technology barrier.Also further carry out for relevant department of China simultaneously
The authenticity supervision of the quality of Manuka honey, source and the name of product marked, the place of production and process is mentioned
For scientific evidence and data basis.It plays a significant role in the work of protection consumer's interests.
Detailed description of the invention
Fig. 1 is hydrogen nuclear magnetic resonance finger-print in embodiment 1.
Fig. 2 is the hydrogen nuclear magnetic resonance map of sample to be tested 1 in embodiment 2.
Fig. 3 is the hydrogen nuclear magnetic resonance map of sample to be tested 2 in embodiment 2.
Fig. 4 is the hydrogen nuclear magnetic resonance map of sample to be tested 3 in embodiment 2.
Fig. 5 is the hydrogen nuclear magnetic resonance map of sample to be tested 4 in embodiment 2.
Specific embodiment
In order to better understand the present invention, we in conjunction with specific embodiments further explain the present invention below
It states.
The determination of 1 characteristic indication object of embodiment
1. instrument and equipment
Experimental facilities includes：400 type Nuclear Magnetic Resonance of Advance（Brooker,Switzerland company）, 14.1 T superconducting magnets, 5 mm
Double-core z- gradient probe and 2.3 controlling test of Topspin and data processing software；5mm nuclear magnetic resonance sample tube；High speed centrifugation
Machine（Sigma, German company）；Turbine mixer（XW-80A type, Instrument Factory, Shanghai Medical Science Univ.）；LP403 assay balance（It matches more
Li Si, German company）；
Test solvent includes：Deuterated water（Deuterium band width is 99.8%）It is purchased from Cambrideg Isotope Laboratories company；
3- trimethylsilyl -1- propyl sulfonic acid sodium（TSPSA）It is purchased from Aldich-Sigma company；Dipotassium hydrogen phosphate and sodium dihydrogen phosphate
（Excellent pure grade）It is purchased from Aldich-Sigma company.
2. honey sample collection
It is collected in Manuka honey, card the slave's card honey, Rui Waruiwa honey, Ka Maxi honey, sage of New Zealand's different sources altogether
7 kinds such as absurd fantastic anthophorids honey, auspicious tower honey, the auspicious honey of Tahoua amount to 114 ceromel samples, and from country of New Zealand
50 commercialization Manuka honeys are analyzed.
3. sample preparation
For commercially available Manuka honey, it is stirred for uniformly, accurately weighing 0.25 g sample in centrifuge tube, 1mL weight is added
Water, dissolution are complete；Above-mentioned 0.8 μ l of solution is taken, the phosphate buffer solution that 100 μ l concentration are 0.5 mol/L is added（pH=2.0）,
3- trimethylsilyl -1- propyl sulfonic acid sodium the inner mark solution and 0.1 mM for being wherein 0.05% containing volume fraction in buffer solution
Sodium azide, vortex oscillation, then with the hydrochloric acid and sodium hydroxide of 1.0 mol/L, adjusts final solution to uniform mixing
PH value is 2.5, take wherein 600 μ l in nuclear magnetic tube.
For ceromel sample, after being stirred for uniformly, is filtered, removed with the nylon filtering cloth that aperture is 0.10mm-0.14mm
In honey after solid impurity, 0.25 g sample is accurately weighed in centrifuge tube, 1mL heavy water is added, and dissolution is complete；It takes above-mentioned molten
The phosphate buffer solution that 100 μ l concentration are 0.5 mol/L is added in 0.8 μ l of liquid（pH=2.0）, volume is wherein contained in buffer solution
The sodium azide of 3- trimethylsilyl -1- propyl sulfonic acid sodium inner mark solution and 0.1 mM that score is 0.05%, vortex oscillation is extremely
Uniformly mixing, then with the hydrochloric acid and sodium hydroxide of 1.0 mol/L, the pH value for adjusting final solution is 2.5, takes wherein 600 μ l
In nuclear magnetic tube.
4. the acquisition of proton magnetic finger-print
Instrument：400 type Nuclear Magnetic Resonance of Advance（Brooker,Switzerland company）, pop one's head in equipped with BBI；Measuring temperature（Probe
Temperature）:20-35 DEG C of room temperature；Ambient humidity: 20-35%;Pulse protocol is：noesygppr1d；Spectrum width: 6410 Hz；
90 ° of pulse widths: pl= 6. 45μs;Pulse delay time: dl= 15 s；Launching centre: O1=4.7；Accumulative frequency: 16
It or is 64.
It is popped one's head in using BBI；Measuring temperature：20-35 DEG C of room temperature；Ambient humidity： 20-35%；400 MHz of observed frequency；
Water peak is suppressed using presaturation method；Pulse protocol is：Noesygppr1d is zg30 or is zgpr；Spectrum width：6410
Hz；90 ° of pulse widths： pl= 6. 45μs；Pulse delay time： dl= 15 s；Launching centre： O1=4.7；Cumulative time
Number：16 or be 64.
114 ceromel samples of different sources, and 50 commercialization Mai Luka from country of New Zealand are measured respectively
The hydrogen nuclear magnetic resonance Spectrum Analysis map of honey, and be superimposed and to form finger-print, as shown in fig. 1.
The characteristic indication object for determining Manuka honey samples is： 1H chemical shift δ be 2.30 ± 0.05ppm, 2.38 ±
Two of 0.05ppm are unimodal.And the criterion for further determining that Manuka honey samples is that unimodal height is high at 2.30ppm
The unimodal height at 2.38ppm, two unimodal relative height ratios are more than or equal to 2.0, and spectral strength error range is no more than
10%。
After measured, limit of identification of this method for Mai Luka characteristic indication object ingredient contained in Manuka honey
It is 10%.
Embodiment 2
By submitted sample respectively marked as 1,2,3,4.
It is pre-processed according to the property of sample, particularly：
For commercially available honey sample, it is stirred for uniformly, accurately weighing 0.25 g sample in centrifuge tube, 1mL heavy water is added,
Dissolution is complete；Above-mentioned 0.8 μ l of solution is taken, the phosphate buffer solution that 100 μ l concentration are 0.5 mol/L is added（pH=2.0）,
3- trimethylsilyl -1- propyl sulfonic acid sodium the inner mark solution and 0.1 mM for being 0.05% containing volume fraction in middle buffer solution
Sodium azide, vortex oscillation, then with the hydrochloric acid and sodium hydroxide of 1.0 mol/L, adjust the pH of final solution to uniform mixing
Value be 2.5, take wherein 600 μ l in nuclear magnetic tube.
For ceromel sample, after being stirred for uniformly, is filtered, removed with the nylon filtering cloth that aperture is 0.10mm-0.14mm
In honey after solid impurity, 0.25 g sample is accurately weighed in centrifuge tube, 1mL heavy water is added, and dissolution is complete；It takes above-mentioned molten
The phosphate buffer solution that 100 μ l concentration are 0.5 mol/L is added in 0.8 μ l of liquid（pH=2.0）, volume is wherein contained in buffer solution
The sodium azide of 3- trimethylsilyl -1- propyl sulfonic acid sodium inner mark solution and 0.1 mM that score is 0.05%, vortex oscillation is extremely
Uniformly mixing, then with the hydrochloric acid and sodium hydroxide of 1.0 mol/L, the pH value for adjusting final solution is 2.5, takes wherein 600 μ l
In nuclear magnetic tube.
The proton magnetic finger-print acquisition of sample to be tested is carried out according to the following conditions
Instrument：400 type Nuclear Magnetic Resonance of Advance（Brooker,Switzerland company）, pop one's head in equipped with BBI；Measuring temperature（Probe
Temperature）:20-35 DEG C of room temperature；Ambient humidity: 20-35%;Pulse protocol is：noesygppr1d；Spectrum width: 6410 Hz；
90 ° of pulse widths: pl= 6. 45μs;Pulse delay time: dl= 15 s；Launching centre: O1=4.7；Accumulative frequency: 16
It or is 64.
It is popped one's head in using BBI；Measuring temperature：20-35 DEG C of room temperature；Ambient humidity： 20-35%；400 MHz of observed frequency；
Water peak is suppressed using presaturation method；Pulse protocol is：Noesygppr1d is zg30 or is zgpr；Spectrum width：6410
Hz；90 ° of pulse widths： pl= 6. 45μs；Pulse delay time： dl= 15 s；Launching centre： O1=4.7；Cumulative time
Number：16 or be 64.
Analyze result：
Chemical shift calibration is carried out to the hydrogen nuclear magnetic resonance Spectrum Analysis spectrogram of 1-4 sample respectively.Spectrogram after calibration is as schemed
Shown in 2-5.Sample 1 does not contain1H chemical shift δ is 2.30ppm and 2.38ppm, therefore sample 1 is judged as Fei Mailuka；Sample
Product 2 exist1H chemical shift δ is at 2.30ppm and 2.38ppm, hence it is evident that it is unimodal containing there are two, and peak height unimodal at 2.30ppm
Higher than the peak height of spectral peak at 2.38ppm, but the ratio of peak at two peaks is lower than 2, therefore sample 2 is judged as Fei Mailuka；3 He of sample
It containing chemical shift δ is obviously two of 2.30ppm and 2.38ppm unimodal in sample 4, the ratio of peak at two peaks is about in sample 3
It is 2.6, the ratio of peak at 4 kinds of two peaks of sample is 3.5, and the ratio of peak that the two samples all meet two peaks is more than or equal to 2.0
It is required that so, sample 3 and sample 4 belong to Manuka honey.
Claims (9)
1. the Manuka honey discrimination method based on nuclear magnetic resonance technique, it is characterised in that：This method is by analyzing test sample to be checked
The NMR spectrum spectral data of product determines whether sample to be tested is Manuka honey, is specifically described as：
A. when spectral analysis of the nuclear magnetic resonance map meets the following conditions simultaneously, which is Manuka honey：
（1）Contain1H chemical shift δ be 2.30 ± 0.05ppm, two of 2.38 ± 0.05ppm it is unimodal；
（2）Unimodal height is higher than unimodal height at 2.38ppm at 2.30ppm, and two unimodal relative height ratios are more than or equal to
2.0；
（3）The error range of spectral peak height is no more than 10%；
B. when spectral analysis of the nuclear magnetic resonance map be unsatisfactory for it is above（1）-（3）When middle either condition, which is not wheat
Lu's card honey.
2. the Manuka honey discrimination method according to claim 1 based on nuclear magnetic resonance technique, which is characterized in that core
The analysis condition of Magnetic Resonance Spectrum is：It is popped one's head in using BBI；Measuring temperature：20-35 DEG C of room temperature；Ambient humidity： 20-35%；
400 MHz of observed frequency；Water peak is suppressed using presaturation method；Pulse protocol is：Noesygppr1d is zg30 or is
zgpr；Spectrum width：6410 Hz；90 ° of pulse widths： pl= 6. 45μs；Pulse delay time： dl= 15 s；Launching centre：
O1=4.7；Accumulative frequency：16 or be 64.
3. the Manuka honey discrimination method according to claim 1 based on nuclear magnetic resonance technique, which is characterized in that core
Magnetic resonance spectroscopy sample preparation methods are：Into honey sample solution, the phosphate that concentration is 0.5-2.0 mol/L is added
Buffer solution, the volume ratio of the two are 800-1500：100-300, vortex oscillation adjust the pH value of solution extremely to uniform mixing
2.5-4.0, take wherein 600 μ l in nuclear magnetic tube.
4. the Manuka honey discrimination method according to claim 3 based on nuclear magnetic resonance technique, which is characterized in that adjustment
The solution of the pH value of solution is hydrochloric acid or sodium hydroxide.
5. the Manuka honey discrimination method according to claim 4 based on nuclear magnetic resonance technique, which is characterized in that hydrochloric acid
Or the concentration of sodium hydroxide is 1.0mol/L.
6. the Manuka honey discrimination method according to claim 3 based on nuclear magnetic resonance technique, which is characterized in that phosphorus
In hydrochlorate buffer solution containing volume fraction be 0.05-0.3% 3- trimethylsilyl -1- propyl sulfonic acid sodium inner mark solution and
The sodium azide of 0.1-3.0 mM.
7. the Manuka honey discrimination method according to claim 3 based on nuclear magnetic resonance technique, which is characterized in that bee
The preparation method of sweet sample solution is：It by the honey sample after thawing, is filtered through nylon filtering cloth, removes solid impurity in honey
Afterwards, 0.25 g sample is accurately weighed in centrifuge tube, 1mL heavy water is added, and dissolution is complete.
8. the Manuka honey discrimination method according to claim 7 based on nuclear magnetic resonance technique, which is characterized in that described
The aperture of nylon filtering cloth is 0.10mm-0.14mm.
9. the Manuka honey discrimination method according to claim 7 based on nuclear magnetic resonance technique, which is characterized in that honey
The thawing processing step of sample is：To the laboratory sample of nodeless mesh, it is stirred for uniformly, to the sample for having crystallization, closed
In the case of, it is placed in the water-bath no more than 60 DEG C and warms, vibrate, stirred evenly after sample all melts, be rapidly cooled to room temperature.
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| RU2696772C1 (en) * | 2019-01-22 | 2019-08-06 | Федеральное государственное автономное образовательное учреждение высшего образования "Северо-Восточный федеральный университет имени М.К.Аммосова" | Method for determining the thermal effect on honey |
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| CN108872289B (en) | 2021-03-02 |
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