Analysis method for distinguishing real honey fromsyrup adulteratedhoney through chromatography mass spectrometry technology in combination with metabonomics method

An analytical method and honey technology, applied in the field of food adulteration identification, can solve the problems of high modeling cost, unsuitable for daily monitoring, and increased use limitations, and achieves low operating technical requirements, simple and fast honey sample pretreatment method, Accurate and reliable test results

Active Publication Date: 2017-09-08
SHANDONG NORMAL UNIV
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  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The sensitivity of nuclear magnetic resonance (NMR) is low, and the metabolites we are concerned about in honey may be ignored, and NMR equipment is expensive and not suitable for daily monitoring
Near-infrared spectroscopy (NIRS) also has its fatal shortcomings: 1. It requires a large number of representative samples with known chemical values ​​to build models
Thus, the analysis of small batches of samples using near-infrared becomes impractical
2. The model needs to be updated continuously. Due to the change of the instrument state or the change of the standard sample, the model will also change accordingly.
3. The model is not universal, and the model of each instrument is different, which increases the limitation of use
4. The cost of modeling is high and the cost of testing is high
The various syrups currently adulterated with honey are very similar to honey in terms of physical and chemical properties, composition and content, and flavor. Therefore, the above-mentioned methods for measuring the quality of honey cannot detect honey adulterated with syrup
[0005] In summary, the existing technology lacks a fast, effective and intuitive method for identifying honey adulteration, and there is no combination of ultra-high performance liquid chromatography-quadrupole-orbitrap high-resolution mass spectrometry combined metabolomics Studies on Determination of Marker Metabolites in Real Honey

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  • Analysis method for distinguishing real honey fromsyrup adulteratedhoney through chromatography mass spectrometry technology in combination with metabonomics method
  • Analysis method for distinguishing real honey fromsyrup adulteratedhoney through chromatography mass spectrometry technology in combination with metabonomics method
  • Analysis method for distinguishing real honey fromsyrup adulteratedhoney through chromatography mass spectrometry technology in combination with metabonomics method

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Effect test

Embodiment 1

[0079] (1) method principle of the present invention:

[0080] After the real honey sample and the syrup-adulterated honey sample were treated with the same pretreatment method, UHPLC was used in series with the Thermo Fisher Q Exactive Mass Spectrometer to realize the separation and determination of the chemical components in the sample, and the Compounds Discoverer software was used to analyze the raw data obtained by the instrument. Chromatographic peak extraction, peak alignment and library search analysis of unknown compounds. Multivariate statistical analysis PCA analysis was used to distinguish real honey from syrup-adulterated honey.

[0081] (2) Sample pretreatment

[0082] Weigh 1g of honey sample (the number of repetitions for one sample is 6 times) into a 50mL centrifuge tube, add 20mL of extractant (the extractant is mixed with equal volumes of methanol containing 1% formic acid and ultrapure water), and vortex to mix the honey sample Completely dissolve, place ...

Embodiment 2

[0102] The method for screening real honey marker metabolites based on UHPLC tandem Thermo Fisher Q Exactive Mass Spectrometer combined with metabolomics method comprises the following steps:

[0103] (1) Sample pretreatment

[0104] Put 1g of real honey sample in a 50mL centrifuge tube, add 20mL extractant (the extractant is mixed with equal volumes of methanol containing 1% formic acid and ultrapure water), vortex and mix until the honey sample is completely dissolved, and place the centrifuge tube in ultrasonic cleaning Sonicate in the machine for 25 minutes, centrifuge at 1000 rpm for 5 minutes, and filter the supernatant with a 0.22 μm organic filter membrane for sample loading.

[0105] Put 1g of syrup sample in a 50mL centrifuge tube, add 20mL of extractant (the extractant is mixed with equal volumes of methanol containing 1% formic acid and ultrapure water), vortex and mix until the syrup sample is completely dissolved, and place the centrifuge tube in an ultrasonic cl...

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Abstract

The invention discloses analysis method for distinguishing realhoney fromsyrup adulteratedhoney througha chromatography mass spectrometry technology in combination with a metabonomics method. The method comprises the following steps: performing pretreatment on a real honey sample and to-be-detectedsyrup adulteratedhoney with the same honey source of real honeyby adoptingan organic solventrespectively, separating and measuring chemical components in the samples subjected to pretreatment through an ultra-high performance liquid chromatography-high resolution mass spectrum, then preprocessing UHPLC-MS original data of the obtained real honey sample and the to-be-detected honey sample, and finally analyzing and distinguishing realhoney fromsyrup adulteratedhoney througha multivariate statistical analysis method PCA. The analysis method is superior to other detection methods, does not need qualitatively and quantificationally measuring one certain or certain targeted matter, and is a macroscopic and non-target method for varietydistinguishment.

Description

technical field [0001] The invention relates to a detection method for distinguishing real honey from syrup-adulterated honey by applying UHPLC-Q Exactive combined metabonomics technology, and belongs to the technical field of food adulteration identification. Background technique [0002] Honey is a natural sweet substance that bees collect nectar, secretions or honeydew from plants, mix with their own secretions, and fully brew. Honey has high nutritional value, but due to the high price and low output of honey, it makes Honey has become a main object of adulteration by illegal traders. In order to improve the production enthusiasm of beekeepers, protect the interests of consumers, support the fair competition of formal honey production enterprises, maintain the order of the honey market, and promote the healthy development of my country's honey industry, therefore It is of great significance and value to find the marker metabolites of real honey samples, so as to try to est...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/14
CPCG01N30/02G01N30/14G01N2030/146
Inventor 耿越祝建华江瑶王骏王凯利宿书芳
Owner SHANDONG NORMAL UNIV
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