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A method for non-directional screening of flavors, fragrances and their derivatives in food based on characteristic fragments of gas mass spectrometry

A flavor, fragrance, and non-directional technology, which is applied in the field of non-directional screening of flavors, fragrances and their derivatives in food based on gas mass spectrometry characteristic fragments, can solve the problems of inaccurate results, increased errors, unknown structures of unknown compounds, etc., and achieves scientific results. Accuracy, low detection cost, and wide screening range

Active Publication Date: 2021-12-24
SOUTH CHINA AGRI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Only a few fragment ions of one standard are used to quantify unknown compounds through the response ratio of mass spectrometry, and the results are not accurate enough
The first difficulty in the quantification of unknown compounds is that the structure of the unknown compound is unknown, and the second difficulty lies in the determination of the number of fragment ions used for quantification. Some ions are interferences, too many will easily increase the error, too few will not be characteristic enough, and the results will not be accurate enough.

Method used

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  • A method for non-directional screening of flavors, fragrances and their derivatives in food based on characteristic fragments of gas mass spectrometry
  • A method for non-directional screening of flavors, fragrances and their derivatives in food based on characteristic fragments of gas mass spectrometry
  • A method for non-directional screening of flavors, fragrances and their derivatives in food based on characteristic fragments of gas mass spectrometry

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0055] Qualitative screening of vanillin in embodiment 1 liquid milk

[0056] 1. Detection of samples to be tested

[0057] Liquid milk: Accurately weigh 5.0 g of liquid milk sample into a 15 mL headspace bottle, add 100 μL of 5 mg / L vanillin compound standard mixture, shake and mix evenly. Add 3g of sodium chloride for GC-Q-TOF determination to obtain the full scan spectrum and data of the sample to be tested.

[0058] Instrument parameter setting:

[0059] Solid phase microextraction conditions: oscillator preheating temperature: 70°C; rotating speed: 500r / min; preheating time: 20min; extraction time: 25min; desorption time: 5min.

[0060] Chromatographic conditions: gas chromatographic column is DB-5MS (30m×0.25mm×0.25μm); temperature program heating process: keep at 80°C for 2min, raise the temperature to 150°C at 10°C / min, keep it for 5min, then raise the temperature to 150°C at 20°C / min 280°C, hold for 3.5min; carrier gas: helium, purity ≥99.999%, flow rate 1.5mL / min;...

Embodiment 2

[0075] Semi-quantitative detection of embodiment 2 vanillin compounds

[0076] 1. Detection of semi-quantitative samples

[0077] Semi-quantitative milk powder sample preparation: Weigh 5.0g of milk powder, add 45mL of water to prepare, weigh 5.0g into a 15mL headspace bottle, add 100μL of 5mg / L vanillin compounds mixed standard, shake and mix well . Add 3g of sodium chloride for GC-Q-TOF determination to obtain the full scan spectrum and data of the sample to be tested.

[0078] Instrument parameter setting:

[0079] Solid phase microextraction conditions: oscillator preheating temperature: 70°C; rotating speed: 500r / min; preheating time: 20min; extraction time: 25min; desorption time: 5min.

[0080] Chromatographic conditions: gas chromatographic column is DB-5MS (30m×0.25mm×0.25μm); temperature program heating process: keep at 80°C for 2min, raise the temperature to 150°C at 10°C / min, keep it for 5min, then raise the temperature to 150°C at 20°C / min 280°C, hold for 3.5m...

Embodiment 3

[0113] Example 3: Semi-quantitative homologues of vanillin

[0114] 1. Detection of semi-quantitative samples

[0115] Semi-quantitative milk powder sample preparation: Weigh 5.0g of milk powder, add 45mL of water to prepare, weigh 5.0g into a 15mL headspace bottle, add 100μL of 5mg / L methyl vanillin and ethyl vanillin compounds Mix the standards and vortex to mix well. Add 3g of sodium chloride for GC-Q-TOF determination to obtain the full scan spectrum and data of the sample to be tested.

[0116] Instrument parameter setting:

[0117] Solid phase microextraction conditions: oscillator preheating temperature: 70°C; rotating speed: 500r / min; preheating time: 20min; extraction time: 25min; desorption time: 5min.

[0118] Chromatographic conditions: gas chromatographic column is DB-5MS (30m×0.25mm×0.25μm); temperature program heating process: keep at 80°C for 2min, raise the temperature to 150°C at 10°C / min, keep it for 5min, then raise the temperature to 150°C at 20°C / min ...

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Abstract

The invention provides a method for non-directional screening of flavors and fragrances and their derivatives in food based on gas phase mass spectrometry characteristic fragments. The mass-to-charge ratio and relative abundance of compound fragment ions are collected through NIST spectral library and standard experiment, and a database is established; the characteristic ion fragments of a class of compounds are calculated by TF‑IDF algorithm, which is used to qualitatively determine whether there is such a compound in unknown samples ; Finally, by calculating the number of fragment ions matching the sample data and the compound in the database, the relative abundance ratio deviation of fragment ions, and the ranking deviation of fragment ions, select the compound that is most similar in structure to the unknown sample, and select the one that matches, and Fragment ions with a relative abundance ≥ 0.1 were used as quantitative ions to make a standard curve for semi-quantitative analysis of unknown samples. The invention has wide screening range and high efficiency, can simultaneously realize the qualitative and semi-quantitative detection of flavors and fragrances and their derivatives in food, and the results are scientific and accurate.

Description

technical field [0001] The invention belongs to the technical field of food detection, and more specifically relates to a method for non-directional screening of flavors and fragrances and their derivatives in food based on gas phase mass spectrometry characteristic fragments. Background technique [0002] Non-directional screening technology is used to determine the possible risk substances in the sample, and is often used in the detection of pesticide and veterinary drug residues in the food field, food safety testing, etc. Among them, mass spectrometer, because of its relatively wide scanning range, can realize the screening, qualitative and quantitative analysis of various chemical substances, and is the most commonly used instrument for data acquisition in non-directional screening methods. Usually, the non-directed method needs to purchase standard products to establish a directed screening database, and then match the collected sample data with the compound informatio...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/06G01N30/88G01N30/86
CPCG01N30/06G01N30/88G01N30/8696
Inventor 韦晓群陈元佳曾广丰梁宇轩刘婕林森煜罗林雷红涛孙远明
Owner SOUTH CHINA AGRI UNIV
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