CN107449836A - The quick discriminating detection method of Manuka honey - Google Patents
The quick discriminating detection method of Manuka honey Download PDFInfo
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- CN107449836A CN107449836A CN201610806572.8A CN201610806572A CN107449836A CN 107449836 A CN107449836 A CN 107449836A CN 201610806572 A CN201610806572 A CN 201610806572A CN 107449836 A CN107449836 A CN 107449836A
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/62—Detectors specially adapted therefor
- G01N30/72—Mass spectrometers
- G01N30/7233—Mass spectrometers interfaced to liquid or supercritical fluid chromatograph
- G01N30/724—Nebulising, aerosol formation or ionisation
- G01N30/7266—Nebulising, aerosol formation or ionisation by electric field, e.g. electrospray
Abstract
The invention belongs to field of food detection, more particularly to a kind of quick discriminating detection method of Manuka honey.Detection method disclosed in the present invention is using high performance liquid chromatography level Four bar electrostatic field orbit trap high resolution mass spectrum as detection means, with 3,5 glucose glycosides of dimethoxy p-methyl 4 pairs are characterized detection mark, can quickly, accurately differentiate Manuka honey.This method integrality is strong, specificity is good, controllability is strong, accuracy is high.The implementation of the present invention can provide technical support for the discriminatory analysis of Manuka honey, protect the legitimate rights and interests of consumers, and for specification bee's product market and promote the sound development of bee product cause to have highly important meaning.
Description
Technical field
The invention belongs to field of food detection, more particularly to a kind of quick discriminating detection method of Manuka honey.
Background technology
Manuka honey is a kind of precious distinctive honey kind of New Zealand, be a kind of distinctive shrub of honeybee collection New Zealand-
What Manuka (Leptospermum scoparium) nectar was brewageed.It is Mai Luka in place of being different from other honey
Honey has powerful and unique antibacterial activity.Honey typically all has antibacterial activity, this be by honey high osmosis in itself, compared with
Strong acidity and caused by typically containing peroxide.And the antibacterial activity of Manuka honey is then independent of peroxide,
Therefore it is referred to as non-peroxidating antibacterial activity (non-peroxide antibacterial activity, NPA).At present, new west
Blue Manuka honey outlet annual growth by 10% or so in the past 10 years, 2013, the honey value 1.28 from New Zealand outlet
Hundred million New Zealand Dollars.But 1700~2000 tons are only about produced every year according to the statistics of one beekeeper association of New Zealand, New Zealand
Manuka honey, and in the world, the honey sold every year with Mai Luka names is up to more than 10,000 tons.Mai Luka honeybees
The behind that honey is largely faked certainly exists the commercial profit of great number.Equally be 500g packaging honey, the price of Manuka honey
More than 10 times of typically domestic honey, typically 50% is also higher by compared with other import honey.Moreover, Activity Rank is got over
Height, price are higher.This is resulted in pretends to be Manuka honey, and false sign Manuka honey to live with syrup or other honey
The phenomenon of property grade is of common occurrence.
In by the end of July, 2014, and New Zealand primary industry portion (MPI) has promulgated portion《Provisional Manuka honey label instructions
Policy》(Interim Labeling Guide for Manuka Honey), is advised to the Product labelling of Manuka honey
Model, and the discriminating to Manuka honey gives provisional standard.Standard provides, only meets color and luster >=62mm
Pfund, conductance：347-867 μ S/cm, flavour：Mineral flavor, slight bitter, smell：Wet soil taste, similar ericophyte smell,
Fragrant odour, there is the pollen of manuka floral and the honeybee of dihydroxyacetone (DHA) (DHA) and methyl-glyoxal (MGO) index can be detected
Honey, " Manuka " printed words could be marked on its Product labelling, however, these indexs can not fundamentally exclude to adulterate,
Adulterated the problem of making vacation.
The content of the invention
The purpose of the present invention is to find a kind of simple, quick and with highly sensitive Manuka honey discriminating detection side
Method.
In order to realize the discriminating of Manuka honey, the present invention uses high performance liquid chromatography-quadrupole rod electrostatic field orbital drive-height
Resolution Mass Spectrometry, by the more pure natural Mai Luka of difference analysis method and the honey of other different nectariferous plants, find out mass number
For 582.2154, molecular structural formula is (C24H38O16) Manuka honey endogenous characteristic indication thing.And according to high resolution mass spectrum
Parent ion accurate mass number and daughter ion fragments characteristic, so as to it is qualitative and quantitatively confirm honey in whether contain Mai Luka honeybees
Sweet characteristic indication thing and its content.
It is Manuka honey to illustrate sample to be detected if following two conditions are met, if be unsatisfactory for following any
One condition, then it is not Manuka honey to illustrate sample to be detected, and the two conditions are respectively：
1st, the double glucose glycosides of 3,5- dimethoxy p-methyls -4- are contained in detected sample；
2nd, the content of the double glucose glycosides of 3,5- dimethoxy p-methyls -4- is more than or equal in detected sample
100mg/kg。
Detection is carried out in three steps altogether, including sample pre-treatments, liquid chromatogram separation and Mass Spectrometer Method.
Specifically, sample pre-treatments are that first honey is dissolved in the water, and stand, take upper solution filter membrane, as entering
All product.
Described filter membrane is aqueous phase filter membrane (0.45um).
More specifically mode of operation is accurately to weigh the sample 1.00g (being accurate to 0.01g) after dissolving first in suitable for it
When graduated vessels in, be then settled to 10.0mL with water, the concussion that is vortexed takes appropriate supernatant liquor filter membrane, obtained to dissolving
Sample introduction sample for analysis.
After obtaining sample introduction sample, we are to further carrying out liquid chromatogram separation and Mass Spectrometer Method, so as to obtain correspondingly
Liquid chromatogram and mass spectrogram.
Meanwhile we further individually disclose more preferably high performance liquid chromatography separation condition and matter in the present invention
Testing conditions are composed, it is specific as follows：
(1) high performance liquid chromatography separation condition is as follows,
Chromatographic column：Dikma Diamonsil Plus C18150*4.6mm chromatographic column；
Mobile phase：A is 0.1% (v/v) aqueous formic acid, and B is acetonitrile；
Flow velocity：0.8mL/min；
Gradient elution program：0-2min 70%A, 2-12min 70-10%A, 12-15min 10%A, 15-16min10-
90%A, 16-18min 70%A；
Column temperature：25℃；
Sampling volume：25μL.
(2) Mass Spectrometer Method is detection ion gun from heatable electric spray ion source, using anion scan pattern, inspection
Survey condition is,
350 DEG C of capillary temperature；
Sheath gas (N2) flow velocity 50L/min；
Aid in gas (N2) flow velocity 6L/min；
Purge gass (N2) flow velocity 3L/min；
Spray voltage is 3KV, lens voltage 50V；
Target-MS2Scan intermediate-resolution R=17500；Maximum residence time：100ms；
Separator window：2.0m/z；Intensity threshold：4×104。
Using 3,5- dimethoxy p-methyls -4- in spectrogram obtained by foregoing preferred high performance liquid chromatography separation condition
The retention time of double glucose glycoside chromatographic peaks is 13.4min or so.
Using in spectrogram obtained by foregoing Mass Spectrometer Method condition, the double glucose of 3,5- dimethoxy p-methyl -4- are sugared
The characteristic ion of glycosides is to being 581.1703m/z for 211.0603m/z and 196.0370m/z, its accurate mass-to-charge ratio of feature parent ion.
Further, we also individually disclose the method that specific Manuka honey differentiates detection, including qualitative and fixed
Measure two steps：
It is first qualitative detection, comprises the following steps：
(1) with the double glucose glycoside standard items of 3,5- dimethoxy p-methyls -4- establish standard liquid chromatograph figure and
Standard mass spectrogram；
(2) detected sample is detected with the condition in step (1), obtain detected sample liquid chromatogram and
Mass spectrogram；
(3) spectrogram that step (1) and (2) obtain is contrasted, if having this in the liquid chromatogram that step (2) obtains
One chromatographic peak of sample, it is differed with standard items appearance time ± 2.5%, and mass number deviation is within 10ppm；Simultaneously in step
Suddenly in the mass spectrogram that (2) obtain, after background correction, it is special to there are the double glucose glycosides of 3,5- dimethoxy p-methyls -4-
Ion pair is levied, and its relative abundance, compared with the relative abundance of the fairly standard product of concentration, its deviation allows relative error in following table
It is interior,
If meeting above-mentioned condition, it is double to enter to show to contain in detected sample 3,5- dimethoxy p-methyls -4-
Glucose glycoside.
Further, it is also necessary to carry out quantitative detecting method, specifically include following steps：
(4) the double glucose glycoside standards of 3,5- dimethoxy p-methyls -4- for preparing one group of concentration known content are molten
Liquid, and using the exact mass chromatographic peak peak area of characteristic ion as ordinate, levels are abscissa, draw standard curve；
(5) standard curve of step (4) is utilized, the exact mass chromatographic peak calculated by peak area obtained with step (2) obtains
The levels of characteristic indication thing in testing sample.
According to quantitative testing result, think that detected sample is wheat if measuring levels and being more than or equal to 100mg/kg
Lu's card honey；If measuring levels is less than 100mg/kg, then it is assumed that the detected sample is not Manuka honey.
In quantitative determination, we are also important to note that if the chromatographic peak peak area that step (5) obtains exceeds standard curve
Scope, testing sample just should be further diluted, until its peak area enters within standard curve range.
Meanwhile the present inventor should also be noted that in quantitative detection, we directly apply what is obtained in step (2)
Liquid chromatogram.If during quantitative detection is used alone, i.e., do not have under the precondition of liquid chromatogram, Wo Menke
With the step of in the centre of step (4) and step (5), one step of increase obtains liquid chromatogram, namely one step of increase and step (2)
Identical step.
The present invention has advantages below：1. sample pre-treatments are simple, reagent is nontoxic, honey sample only needs to be dissolved in water
Chromatograph mass spectrum analysis can be carried out；2. analysis time is short, the analysis time of whole sample only needs 18 minutes, for high-throughout
Analysis detection, substantially reduces detection cycle；3. sensitivity and accuracy are high, relative to other detection methods, the inventive method
Used instrument is high resolution mass spectrum, can reach higher sensitivity, by the abundance for comparing parent ion and fragment ion
Than improving the accuracy of detection.The method of the invention can make up the defects of current Manuka honey discrimination method is present.
The present invention is originally indicated using the double glucose glycosides of 3,5- dimethoxy p-methyls -4- as detection
Thing, can effectively solve the problems, such as current Manuka honey can not quick discriminating it is quantitative, protect consumer legitimate right, for
Specification bee's product market and propulsion mouth honey product develop in a healthy way and have highly important meaning.
Brief description of the drawings
Fig. 1 is the extraction ion stream chromatogram of the double glucose glycoside standard liquids of 3,5- dimethoxy p-methyls -4-；
Fig. 2 is the extraction ion of the double glucose glycosides of 3,5- dimethoxy p-methyls -4- in actual detected sample
Flow chromatography figure；
Fig. 3 is that the two level of the double glucose glycosides of 3,5- dimethoxy p-methyls -4- in actual detected sample is swept entirely
Retouch mass spectrogram.
Embodiment
In order to be better understood from the present invention, below we in conjunction with specific embodiments to the present invention further explained
State.
The investigation and foundation of the liquid chromatogram of embodiment 1, mass spectrometry method
Standard items and reagent used are in the embodiment：The double glucose glycosides of 3,5- dimethoxy p-methyl -4- are pure
Degree is more than 99%；Experiment is purchased from German Merck companies with acetonitrile (chromatographically pure)；Formic acid (chromatographically pure) comes from TEDIA companies of the U.S..
Appropriate standard substance is accurately weighed, 1.0mg/mL standard reserving solution is made into water, is stored for 4 DEG C in refrigerator.With
Acetonitrile water (1:9v/v) it is diluted to the working solution that concentration is 100 μ g/ml.
1. the foundation of liquid phase chromatogram condition
A small amount of formic acid is added during liquid phase analysis.
High-efficient liquid phase chromatogram condition is as follows：
Chromatographic column：Dikma Diamonsil Plus C18150*4.6mm chromatographic column；
Mobile phase：A is 0.1% (v/v) aqueous formic acid, and B is acetonitrile；
Flow velocity：0.8mL/min；
Gradient elution program：Gradient elution program：0-2min 70%A, 2-12min 70-10%A, 12-15min 10%
A, 15-16min 10-90%A, 16-18min 70%A, remaining content are B；
Column temperature：25℃；
Sample size：25μL.
2. the foundation of Mass Spectrometry Conditions:
Target compound criteria solution is directly injected into mass spectrograph with flow injection mode (FIA), carries out full scan detection,
Obtain one-level quasi-molecular ion peak [M-H]-, using the most commonly used electron spray ionisation source (ESI-) to feature mark in mass spectral analysis
Will thing carries out the optimization of spray voltage, collision energy, atomising air amount, final choice [M-H]-Surveyed as target compound
It is fixed.The most strong parent ion of signal intensity and two level daughter fragment ion are chosen respectively simultaneously as qualitative and quota ion, it is final excellent
Qualitative and quota ion after change is shown in Table 1, and the extraction ion flow graph of standard liquid is as shown in Figure 1.
The Information in Mass Spectra table of table 1
Testing conditions are,
350 DEG C of capillary temperature；
Sheath gas (N2) flow velocity 50L/min；
Aid in gas (N2) flow velocity 6L/min；
Purge gass (N2) flow velocity 3L/min；
Spray voltage is 3KV, lens voltage 50V；
Target-MS2Scan intermediate-resolution R=17500；Maximum residence time：100ms；
Separator window：2.0m/z；Intensity threshold：4×104。
The measure of the double glucose glycoside contents of 3,5- dimethoxy p-methyls -4- in the honey of embodiment 2
1. the content analysis of the double glucose glycosides of 3,5- dimethoxy p-methyls -4- in Manuka honey
The accurate sample 1.0g (being accurate to 0.01g) weighed after melting is settled to 10.0mL into volumetric bottle with water, is vortexed
To dissolving, appropriate supernatant liquor filter membrane is taken, prepares sample introduction analysis.
Detection method in Application Example 1 detects to 127 Manuka honeys taken out from honeycomb, as a result shows
Show the content of the double glucose glycosides of 3,5- dimethoxy p-methyls -4- in 127 Manuka honeys in 112.3-
Between 998.7mg/kg.As can be seen from the results, 3,5- dimethoxybenzoic acid first is contained in 127 Manuka honeys
This characteristic indication thing of the double glucose glycosides of ester -4-, and content is more than or equal to 100mg/kg.
2. the analysis of the double glucose glycoside contents of 3,5- dimethoxy p-methyls -4- in other non-Manuka honeys
To the Ka Luka honey from New Zealand's different sources, Rui Waruiwa honey, Karma wish honey, Christmas flower honey,
Auspicious tower honey, the auspicious honey of Tahoua amount to 68 samples, and from the Xinjiang of China, Inner Mongol, Henan, Jiangsu, Shandong, Liaoning, four
Rape, acacia, lime tree, the twigs of the chaste tree and the sunflower on the ground such as river, Jilin, Shaanxi, Hubei and Hebei amount to 93 natural honey samples and entered
Detection is gone.
As a result find that the double glucose glycoside contents of 3,5- dimethoxy p-methyls -4- are equal in Chinese 93 honey samples
Less than method detection limit 10mg/kg.There are 6 samples 3,5- dimethoxybenzoic acid first in Zelanian 68 honey samples
For the double glucose glycoside contents of ester -4- between 10-65mg/kg, remaining 62 sample standard deviation is less than method detection limit 10mg/kg, examines
The reason for considering the miscellaneous nectar of 6 New Zealand honey samples with the presence of detection causes 3,5- dimethoxy p-methyls -4- double
Glucose glycoside has detection, but content is not above 100mg/kg, therefore the double glucose of 3,5- dimethoxy p-methyl -4-
Glucosides is more than or equal to 100mg/kg as Manuka honey mark and content, can be used as and judge the honey sample for Mai Luka
The efficiency index of honey.
Embodiment 33, the double glucose glycosides of 5- dimethoxy p-methyls -4- are as Manuka honey characteristic indication thing
Methodological study
Standard reserving solution acetonitrile water (1:Standard working solution 9v/v) is diluted to, obtains content successively as 1.0 μ g/mL, 5.0
μ g/mL, 10.0 μ g/mL, 20.0 μ g/mL, 50.0 μ g/mL and 100.0 μ g/mL standard liquid, are determined, external standard by following condition
Standard measure.
(1) high performance liquid chromatography separation condition is as follows,
Chromatographic column：Dikma Diamonsil Plus C18150*4.6mm chromatographic column；
Mobile phase：A is 0.1% (v/v) aqueous formic acid, and B is acetonitrile；
Flow velocity：0.8mL/min；
Gradient elution program：0-2min 70%A, 2-12min 70-10%A, 12-15min 10%A, 15-16min10-
90%A, 16-18min 70%A；
Column temperature：25℃；
Sampling volume：25μL.
(2) Mass Spectrometer Method is detection ion gun from heatable electric spray ion source, using anion scan pattern, inspection
Survey condition is,
350 DEG C of capillary temperature；
Sheath gas (N2) flow velocity 50L/min；
Aid in gas (N2) flow velocity 6L/min；
Purge gass (N2) flow velocity 3L/min；
Spray voltage is 3KV, lens voltage 50V；
Target-MS2Scan intermediate-resolution R=17500；Maximum residence time：100ms；
Separator window：2.0m/z；Intensity threshold：4×104。
It is abscissa using the exact mass chromatographic peak area of characteristic ion as ordinate, content, draws standard curve, standard
Curve is：Y=1.6e5x+1021, coefficient correlation (r) are more than 0.99, show the linear relationship in the range of 1.0~100.0 μ g/mL
Well.
50,100 and 200mg/kg3 are added in 3 kinds of honey samples such as Manuka honey, Ka Luka honey and poplar Chinese scholartree honey
The horizontal standard reserving solution of different mark-ons, each level is according to aforementioned condition liquid chromatogram and Mass Spectrometer Method condition replication 6
It is secondary.Average recovery rate scope is between 86-95%, and relative standard deviation scope is between 3.2-5.8%.
Illustrate that the double glucose glycosides of 3,5- dimethoxy p-methyls -4- are steady as Manuka honey characteristic indication thing
It is fixed, reliable.
The discriminating detection of the honey sample to be detected of embodiment 4
1. qualitative detection
Honey sample to be detected is subjected to sample treatment and high-efficient liquid phase color according to the method disclosed in embodiment 1 and 3
Spectrum-level Four bar electrostatic field orbit trap high resolution mass spectrum detection, obtains mass spectrogram as shown in Figure 2, with the standard spectrogram pair in Fig. 1
Than using relative retention time and accurate mass number and secondary fragment as qualitative foundation.
This in Fig. 13, the retention time of the double glucose glycosides of 5- dimethoxy p-methyls -4- is about 13.92min, figure
The chromatographic peak retention time detected in 2 in sample is 13.4min or so, with quasi- condition difference within ± 2.5%, mass number deviation
Within 10ppm.Therefore, we are further investigated under the conditions of above-mentioned chromatography-mass spectroscopy, selected two couple after background correction
The uniformity of ion pair and the relative abundance of the fairly standard solution of concentration.The m z of mark is in standard mass spectrogram
581.1703, daughter ion is 211.0603 and 196.0370/32, mass spectral results as disclosed in fig. 3, and combines following table：
| Relative ion abundance (% base peaks) | ＞ 50% | ＞ 20% to 50% | ＞ 10% to 20% | ≤ 10% |
| The relative error of permission | ± 20% | ± 25% | ± 30% | ± 50% |
We have seen that the relative abundance of testing sample its in the relative error of permission, can determine whether testing sample in this example
Containing Manuka honey characteristic indication thing 3, the double glucose glycosides of 5- dimethoxy p-methyls -4-.
Further, we carry out content investigation to it.
2. quantitative detection
The formulation of standard curve
Compound concentration scope is 1.0~100.0 μ g/mL standard liquid, by the method sample introduction in embodiment 1, with peak face
Product makees linear regression to concentration, and its concentration has good linear relationship with response, and linear equation is y=5.18 × 106x+
1.67×103, correlation R2For more than 0.999.
The peak area of Fig. 2 Plays materials is calculated, using equation of linear regression, obtains 3,5- dimethoxy benzenes first in honey
The concentration of the double glucose glycosides of sour methyl esters -4- is 321mg/kg, more than 100mg/kg.
Aggregate qualitative and quantitative testing result, the testing sample are qualified Manuka honey.
Claims (7)
1. the quick discriminating detection method of Manuka honey, it is characterized in that with high performance liquid chromatography-level Four bar electrostatic field orbit trap
High resolution mass spectrum is detection means, and detection mark is characterized with the double glucose glycosides of 3,5- dimethoxy p-methyls -4-.
2. the quick discriminating detection method of Manuka honey according to claim 1, it is characterized in that, high performance liquid chromatography point
It is as follows from condition：
Chromatographic column：Dikma Diamonsil Plus C18150*4.6mm chromatographic column；
Mobile phase：A is 0.1% (v/v) aqueous formic acid, and B is acetonitrile；
Flow velocity：0.8mL/min；
Gradient elution program：0-2min 70%A, 2-12min 70-10%A, 12-15min 10%A, 15-16min 10-
90%A, 16-18min 70%A；
Column temperature：25℃；
Sampling volume：25μL.
3. the quick discriminating detection method of Manuka honey according to claim 1, it is characterized in that, Mass Spectrometer Method is selected can
The electric spray ion source of heating is detection ion gun, using anion scan pattern, 350 DEG C of capillary temperature.
4. Manuka honey quick discriminating detection method according to claim 1, it is characterized in that, honey sample to be detected
Preparation method is that first honey is dissolved in the water, and is stood, and takes upper solution filter membrane, as sample introduction sample.
5. the quick discriminating detection method of Manuka honey according to claim 2, it is characterized in that, 3,5- dimethoxy benzenes
The retention time of the double glucose glycoside feature detection mark chromatographic peaks of methyl formate -4- is 13.4min or so.
6. the quick discriminating detection method of Manuka honey according to claim 3, it is characterized in that, mark 3,5- diformazans
The accurate mass-to-charge ratio of feature parent ion of the double glucose glycosides of p-methoxybenzoic acid methyl esters -4- is 581.1703m/z, and two level daughter ion is smart
True mass-to-charge ratio is 211.0603m/z and 196.0370m/z.
7. the quick discriminating detection method of Manuka honey as claimed in any of claims 1 to 6, it is characterized in that,
Comprise the following steps：
(1) standard liquid chromatograph figure and standard are established with the double glucose glycoside standard items of 3,5- dimethoxy p-methyls -4-
Mass spectrogram；
(2) detected sample is detected with the condition in step (1), obtains the liquid chromatogram and mass spectrum of detected sample
Figure；
(3) spectrogram that step (1) and (2) obtain is contrasted, if having such one in the liquid chromatogram that step (2) obtains
Individual chromatographic peak, it is differed with standard items appearance time ± 2.5%, and mass number deviation is within 10ppm；Simultaneously in step
(2) in the mass spectrogram obtained, after background correction, the double glucose glycoside features of 3,5- dimethoxy p-methyls -4- be present
Ion pair, and its relative abundance, compared with the relative abundance of the fairly standard product of concentration, its deviation allows in relative error in following table,
If meeting above-mentioned condition, further follow the steps below：
(4) standard liquid of the double glucose glycosides of 3, the 5- dimethoxy p-methyls -4- of preparation concentration known content, and with
The exact mass chromatographic peak peak area of its characteristic ion is ordinate, and levels are abscissa, draws standard curve；
(5) standard curve of step (4) is utilized, the exact mass chromatographic peak calculated by peak area obtained with step (2) obtains to be measured
The levels of the double glucose glycosides of 3,5- dimethoxy p-methyls -4- in sample；
Think that detected sample is qualified Manuka honey if measuring levels and being more than or equal to 100mg/kg；
If measuring levels is less than 100mg/kg, then it is assumed that the detected sample is unqualified Manuka honey.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108120786A (en) * | 2018-01-17 | 2018-06-05 | 山东出入境检验检疫局检验检疫技术中心 | The detection method of methyl-glyoxal in a kind of honey |
| CN109270182A (en) * | 2018-11-28 | 2019-01-25 | 海峡两岸农产品检验检疫技术厦门中心 | A kind of discrimination method of Manuka honey |
| CN109946406A (en) * | 2019-04-15 | 2019-06-28 | 许昌学院 | A kind of true and false method of identification lime tree honey |
| CN111220763A (en) * | 2020-04-24 | 2020-06-02 | 中国农业科学院蜜蜂研究所 | Application of high-content DSM as characteristic marker of linden honey |
| CN114487237A (en) * | 2022-01-26 | 2022-05-13 | 中山奕安泰医药科技有限公司 | Detection method of 3, 5-dimethoxybenzoic acid methyl ester |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2013061816A (en) * | 2011-09-13 | 2013-04-04 | Fujitsu Ltd | Program, information processor, and abnormality determination method |
| US20140274931A1 (en) * | 2011-10-27 | 2014-09-18 | Yoji Kato | Novel compound contained in manuka honey and use of same |
-
2016
- 2016-09-06 CN CN201610806572.8A patent/CN107449836A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2013061816A (en) * | 2011-09-13 | 2013-04-04 | Fujitsu Ltd | Program, information processor, and abnormality determination method |
| US20140274931A1 (en) * | 2011-10-27 | 2014-09-18 | Yoji Kato | Novel compound contained in manuka honey and use of same |
Non-Patent Citations (4)
| Title |
|---|
| YOJI KATO等: "Competitive immunochromatographic assay for leptosperin as a plausible authentication marker of manuka honey", 《FOOD CHEMISTRY》 * |
| YOJI KATO等: "Identification of a Novel Glycoside, Leptosin, as a Chemical Marker of Manuka Honey", 《JOURNAL OF AGRICULTURAL AND FOOD CHEMISTRY》 * |
| YOJI KATO等: "Immunochemical Authentication of Manuka Honey Using a Monoclonal Antibody Specific to a Glycoside of Methyl Syringate", 《JOURNAL OF AGRICULTURAL AND FOOD CHEMISTRY》 * |
| YOJI KATO等: "Plausible Authentication of Manuka Honey and Related Products by Measuring Leptosperin with Methyl Syringate", 《JOURNAL OF AGRICULTURAL AND FOOD CHEMISTRY》 * |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108120786A (en) * | 2018-01-17 | 2018-06-05 | 山东出入境检验检疫局检验检疫技术中心 | The detection method of methyl-glyoxal in a kind of honey |
| CN108120786B (en) * | 2018-01-17 | 2020-06-19 | 山东出入境检验检疫局检验检疫技术中心 | Method for detecting methylglyoxal in honey |
| CN109270182A (en) * | 2018-11-28 | 2019-01-25 | 海峡两岸农产品检验检疫技术厦门中心 | A kind of discrimination method of Manuka honey |
| CN109946406A (en) * | 2019-04-15 | 2019-06-28 | 许昌学院 | A kind of true and false method of identification lime tree honey |
| CN111220763A (en) * | 2020-04-24 | 2020-06-02 | 中国农业科学院蜜蜂研究所 | Application of high-content DSM as characteristic marker of linden honey |
| CN114487237A (en) * | 2022-01-26 | 2022-05-13 | 中山奕安泰医药科技有限公司 | Detection method of 3, 5-dimethoxybenzoic acid methyl ester |
| CN114487237B (en) * | 2022-01-26 | 2023-10-20 | 中山奕安泰医药科技有限公司 | Detection method of 3, 5-dimethoxy methyl benzoate |
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