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

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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

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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

Example Embodiment

[0067] (4) Preparation of sample solution

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

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

Example Embodiment

[0103] Example 1. Optimization of experimental method

[0104] (1) Optimization of pre-processing methods

[0105] ①Optimization of extraction conditions

[0106] The three targets are easily soluble in polar organic solvents such as ether, alcohols, acetone, ethyl acetate, acetonitrile, etc. The literature reported that the extraction solvents analyzed by gas chromatography mostly use ether. However, most food matrices contain a lot of fat and other substances, which are easily soluble in ether. These substances will contaminate the chromatographic column and require additional purification methods to remove these substances for detection; if alcohol solvents are used, the water in the food will be dissolved. The moisture in alcohol is difficult to remove. Sugars and salts will enter the extract with the moisture, causing serious contamination of the instrument. Alcohol solvents may also react with acid anhydride derivative reagents; acetone and ethyl acetate are harmful to fats an...

Example Embodiment

[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 solutions of the three substances into a mixed standard working solution of 0.04, 0.10, 0.20, 1.0, 2.0, 5.0 μg / mL and add 10 μL of the derivatization reagent solution. After derivatizing at 60°C for 20 minutes Cool down to room temperature and inject samples under the best condition of the instrument. Use the integrated area of ​​each compound quantitative ion as the ordinate (Y) and the concentration of each compound (X, μg / mL) as the abscissa to plot The linear equation and linear correlation coefficient r of the three target compounds in this concentration range show that within the concentration range of 0.04~10μg / mL, the concentration of the three compounds has a good linear relationship with the integrated area of ​​the quantification ion. See the specif...

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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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