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A method for the determination of methyl vanillin and ethyl vanillin in milk powder using headspace-solid phase microextraction

A technology of methyl vanillin and ethyl vanillin, which is applied in the direction of measuring devices, instruments, scientific instruments, etc., can solve the problems of high detection limit, cumbersome steps, and low recovery rate, so as to avoid false positives and improve sensitivity , the effect of a wide range of application prospects

Inactive Publication Date: 2016-07-06
INSPECTION & QUARANTINE TECH CENT OF GUANGDONG ENTRY EXIT INSPECTION & QUARANTINE BUREAU
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The above methods all need to use a large amount of organic solvents for extraction, the steps are cumbersome and the recovery rate is low
Gas chromatography, spectrophotometry, high performance liquid chromatography, etc. have the disadvantages that the detection limit is too high and false positives are prone to occur.
There is no report on the simultaneous determination of vanillin and ethyl vanillin in milk powder by headspace solid-phase microextraction-gas chromatography-mass spectrometry

Method used

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  • A method for the determination of methyl vanillin and ethyl vanillin in milk powder using headspace-solid phase microextraction
  • A method for the determination of methyl vanillin and ethyl vanillin in milk powder using headspace-solid phase microextraction
  • A method for the determination of methyl vanillin and ethyl vanillin in milk powder using headspace-solid phase microextraction

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0071] Embodiment 1: selection experiment of extraction fiber type

[0072] According to the principle of similar miscibility, the non-polar fiber coating has a higher extraction efficiency for non-polar compounds, while the polar fiber coating has a higher extraction efficiency for polar compounds. Under the conditions of 70°C, oscillator speed 500r / min, equilibration 10min, and headspace solid-phase microextraction 20min, the extraction effects of 7 different types of extraction fibers on the matrix standard mixture were investigated. figure 1 It is a comparison chart of the extraction effects of 7 different types of extraction fibers on the matrix standard mixture. The extraction capabilities of the seven extraction fibers were compared from three aspects: the amount of extracted methyl vanillin and ethyl vanillin (expressed by peak area), the resolution of chromatographic peaks and the peak shape. figure 1 The results show that: the peaks of the target components obtained...

Embodiment 2

[0073] Embodiment 2: Optimization experiment of balance time

[0074] Preheat the sample to achieve gas-liquid equilibrium. Controlling other conditions unchanged, the test investigated the peak area changes of methyl vanillin and ethyl vanillin when the equilibrium time was 10, 20, 30, 40, and 50 min respectively. figure 2 It is the graph of the optimization experiment result of the equilibration time. Such as figure 2 As shown in the results, within the investigated time, the peak area of ​​the target compound increases with time. When the equilibration time is longer than 40min, increasing the equilibration time, the increase of the peak area does not change much, indicating that the equilibration is 40min, and the gas-liquid equilibrium has been reached. Therefore, 40min was chosen as the optimal equilibration time.

Embodiment 3

[0075] Embodiment 3: Optimization experiment of oscillator speed

[0076] Controlling other conditions unchanged, the effects of 250, 400, 500, 600, and 700 r / min on the peak area of ​​the target compound were investigated respectively. image 3 is the graph of the optimized experimental results of the oscillator speed, by image 3 It can be seen that the larger the rotational speed, the larger the target peak area. This is because increasing the stirring speed can not only accelerate the speed of the extracted substance entering the gas phase, but also strengthen the flow of the upper gas, which is beneficial to the transfer of the extracted substance in the gas and improves the extraction efficiency of the analyte. After the rotational speed is greater than 500r / min, the peak area basically no longer shows an increasing state, so this method selects a rotational speed of 500r / min.

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Abstract

The invention provides a method for determining methyl vanillin and ethyl vanillin in milk powder by adopting a headspace-solid phase microextraction technology. The method comprises the following steps: (1) pretreating a sample; (2) performing headspace-solid phase microextraction: sealing a bottle opening of a headspace bottle, oscillating at rotating speed of 250-700 r / min with a balance time of 10-50min, inserting an extracting head into the headspace bottle, extracting at temperature of 40-90 DEG C for 10-50min; and (3) performing gas chromatography-mass spectrum: inserting the extracting head in a sample inlet of a gas chromatograph-mass spectrometer, starting a data acquirer to acquire data, and desorbing at temperature of 240-270 DEG C for 2-6min. The method for determining methyl vanillin and ethyl vanillin in milk powder, established in the invention, is simple and convenient, has the advantages of preventing a false positive result and improving the sensitivity, and has certain practical significance and wide application prospect.

Description

technical field [0001] The invention belongs to the detection field of food additives, and in particular relates to a method for measuring methyl vanillin and ethyl vanillin in milk powder by using a headspace-solid phase microextraction technique. Background technique [0002] Vanillin is an important flavor and fragrance additive in the food industry, mainly including methyl-vanillin (3-methoxy-4-hydroxybenzaldehyde) and ethyl-vanillin (3-ethoxy -4-hydroxybenzaldehyde), whose structural formula is shown below, is widely used as a food flavoring agent because of its vanilla aroma and strong milky aroma. [0003] [0004] At present, there is no national standard determination method for food, only the limit standard for vanillin. The national standard GB2760-2011 stipulates that no flavors and fragrances should be added to infant formula for 0-6 months. Methyl vanillin, ethyl vanillin and vanilla bean extract can be used in formula food for older infants and young chil...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/02G01N30/08
Inventor 王志元韦晓群曾广丰陈文锐易蓉丁博黎海超
Owner INSPECTION & QUARANTINE TECH CENT OF GUANGDONG ENTRY EXIT INSPECTION & QUARANTINE BUREAU
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