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Method used for simultaneous measurement of vanillin, methyl vanillin, and ethyl vanillin in food

A technology of ethyl vanillin and methyl vanillin, applied in the field of detection, can solve the problems of long operation time, less instrument configuration, low efficiency, etc., and achieve the effects of mild derivatization conditions, little matrix interference, and simple pretreatment.

Inactive Publication Date: 2018-02-09
大连市食品检验所
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, for illicitly used sample matrices, only chromatographic-mass spectrometry is sensitive enough to meet food safety regulatory requirements
The food matrix is ​​complex, and it is easy to encounter interference compared with mass spectrometry chromatography, while the instruments used in liquid chromatography-mass spectrometry are more expensive, and there are few such instruments in grassroots laboratories and production enterprises in my country, so it is not easy to promote
In addition, the pretreatment methods reported in the literature mostly use toxic and volatile organic solvents such as ether for extraction, and some use headspace solid-phase microextraction, etc.
Commonly used purification methods include liquid-liquid distribution purification, solid phase extraction purification, etc., and sometimes protein precipitation is required. Most of these methods take a long time to operate, have low efficiency, are prone to false positives, and have a greater risk of harm to the operator. Some special equipment is required
Relevant food matrices are mainly concentrated in dairy products, etc., but there are no methods reported for grains, vegetable oils, etc., and there is no method for simultaneous determination of these three substances by GC-MS

Method used

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  • Method used for simultaneous measurement of vanillin, methyl vanillin, and ethyl vanillin in food
  • Method used for simultaneous measurement of vanillin, methyl vanillin, and ethyl vanillin in food
  • Method used for simultaneous measurement of vanillin, methyl vanillin, and ethyl vanillin in food

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Experimental program
Comparison scheme
Effect test

preparation example Construction

[0067] (4) Preparation of sample solution

[0068] ①Infant milk powder, cereal supplementary food for infants and young children, infant formula milk powder, and grain samples Weigh 2 g of the pretreated sample, add 5 mL of water, then add 10 mL of acetonitrile, vortex for 30 s, and ultrasonically extract at room temperature for 20 min , then add 2 g sodium chloride, shake vigorously for 30 s, sonicate for 10 min, vortex mix, centrifuge at 5 000 r / min for 2 min, take 2 mL of the upper layer extract into a ground glass centrifuge tube with stopper, add 1 mL of n-hexane and 20 μL of derivatization reagent solution and vortexed for 10 s, derivatized at 60 °C for 10 min, cooled to room temperature, added 200 mg of anhydrous magnesium sulfate and vortexed for 20 s, centrifuged at 5 000 r / min After 1 min, remove the lower layer of acetonitrile and filter it with a microporous membrane (0.22 μm, organic phase) before testing.

[0069] ② Weigh 5 g of liquid milk (pasteurized milk, st...

example 1

[0103] Example 1, optimization of experimental method

[0104] (1) Optimization of the pre-processing method

[0105] ① Optimization of extraction conditions

[0106] The three target substances are easily soluble in polar organic solvents such as ether, alcohols, acetone, ethyl acetate, acetonitrile, etc., and ether is mostly used as the extraction solvent for gas chromatography analysis in literature reports. However, most food matrices contain more fat and other substances, which are easily soluble in ether. These substances will contaminate the chromatographic column, and additional purification methods are required to remove these substances before detection can be performed; if alcohol solvents are used, the water in the food will be dissolved. Moisture in alcohol is difficult to remove, sugar and salt will enter the extraction solution with water, causing serious pollution of the instrument, alcohol solvents may also react with anhydride derivative reagents; acetone an...

example 2

[0114] Example 2, method verification experiment of the present invention

[0115] (1) Linear range and correlation coefficient

[0116] Use the acetonitrile solution containing the sample matrix to prepare the standard stock solution of the three substances into a mixed standard working solution of 0.04, 0.10, 0.20, 1.0, 2.0, and 5.0 μg / mL, and add 10 μL of derivatization reagent solution, after derivatization at 60 ° C for 20 min Cool to room temperature, inject samples separately under the optimal state of the instrument, take the integrated area of ​​the quantified ion of each compound as the ordinate (Y), and the concentration of each compound (X, μg / mL) as the abscissa to draw a graph to obtain The linear equations and linear correlation coefficient r of the three target compounds in this concentration range show that within the concentration range of 0.04-10 μg / mL, the linear relationship between the concentration of the three compounds and the integral area of ​​their ...

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Abstract

The invention discloses a method used for simultaneous measurement of vanillin, methyl vanillin, and ethyl vanillin in food. According to the method, measurement of vanillin and ethyl vanillin is carried out after conversion of vanillin and ethyl vanillin into propionates via derivatization. The method comprises following steps: solution preparation, standard stock solution preparation, sample solution preparation, gas chromatography-mass spectrometry qualitative analysis, and quantitative determination. The method can be used for simultaneous measurement of vanillin, methyl vanillin, and ethyl vanillin in cereal grains, liquid milk, single cream, plant oil, and infant formula foods; propionic anhydride derivatization is adopted; detection efficiency is high; detection cost is low; and themethod is rapid and simple, is high in efficiency, and is convenient to popularize.

Description

technical field [0001] The invention relates to a detection method. Especially a method for the simultaneous determination of vanillin, methyl vanillin and ethyl vanillin in food, mainly used in grains, liquid milk, cream, vegetable oil, infant formula Determination method of base vanillin and ethyl vanillin. Background technique [0002] Vanillin, methyl vanillin and ethyl vanillin all have strong milk flavor, among which vanillin naturally exists in many plants in nature, and the latter two are chemically synthesized substances. The three substances are commonly used food flavor enhancers in food, and they are widely used in candies, biscuits, pastries and beverages. However, it has been reported in the literature that large doses of vanillin can cause headaches, nausea, vomiting, dyspnea, and even liver and kidney damage. However, many merchants in our country illegally add spices in order to pursue the maximum benefit, and even the incidents of "flavored rice" and "fl...

Claims

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Application Information

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IPC IPC(8): G01N30/88G01N30/06
CPCG01N30/06G01N30/88
Inventor 张敬波姜俊毛希琴戴学东曲宝成李鹏余魏
Owner 大连市食品检验所
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