Gas chromatography detection method of corrosion removers in food

A technology of gas chromatography and detection method, which is applied in the detection field of gas chromatography for determination of various preservatives in food, can solve the problems of high requirements for gas chromatography-mass spectrometry instruments, unsuitable promotion and use, and influence on accurate quantification, etc., and achieves detection sensitivity. High, linear, and easy-to-use results

Active Publication Date: 2013-03-27
浙江公正检验中心有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although liquid chromatography and liquid chromatography-mass spectrometry can simultaneously determine a variety of preservatives, due to the variety of food sample matrices, the matrix impurities will cause interfer

Method used

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  • Gas chromatography detection method of corrosion removers in food
  • Gas chromatography detection method of corrosion removers in food
  • Gas chromatography detection method of corrosion removers in food

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0070] Determination of preservatives in soy sauce

[0071] Weigh 5.00g of soy sauce (accurate to 0.01g) into a 125mL separatory funnel, add 10mL of saturated NaCl aqueous solution and 1.0mL of hydrochloric acid solution and mix well, then add 1.0mL of undecanoic acid internal standard solution, and then use 50mL, 30mL, 30mL of Extract three times with diethyl ether, combine the ether layers, wash with 30mL saturated NaCl aqueous solution until neutral, dehydrate through anhydrous sodium sulfate, concentrate in a water bath at 40±2°C to 0.3-0.5mL, blow dry with nitrogen, and dilute to 5.0 mL with acetone mL. After the sample liquid passes through a 0.45 μm filter membrane, it enters the gas chromatograph for determination, and the spectrum is shown in figure 2 , the soy sauce contains propionic acid 0.034g / kg, dimethyl fumarate 0.010g / kg, dehydroacetic acid 0.082g / kg, sorbic acid 0.67g / kg, benzoic acid 0.40g / kg.

Embodiment 2

[0073] Determination of preservatives in orange juice beverages

[0074] Weigh 10.00g of orange juice drink (accurate to 0.01g) into a 125mL separatory funnel, add 10mL saturated NaCl aqueous solution and 1.0mL hydrochloric acid solution and mix well, then add 1.0mL undecanoic acid internal standard solution, and then use 50mL, 30mL, Extract three times with 30 mL of diethyl ether, combine the ether layers, wash with 30 mL of saturated NaCl aqueous solution to neutrality, dehydrate through anhydrous sodium sulfate, concentrate in a water bath at 40±2°C to 0.3-0.5 mL, blow dry with nitrogen, and dilute to 0.3-0.5 mL with acetone. 5.0mL. After the sample liquid passes through a 0.45 μm filter membrane, it enters the gas chromatograph for determination, and the spectrum is shown in image 3 , the beverage contained 0.10g / kg of benzoic acid.

Embodiment 3

[0076] Determination of preservatives in vinegar

[0077] Weigh 7.00g vinegar (accurate to 0.01g) into a 125mL separatory funnel, add 10mL saturated NaCl aqueous solution and 1.0mL hydrochloric acid solution and mix well, then add 1.0mL undecanoic acid internal standard solution, and then use 50mL, 30mL, 30mL Extract three times with diethyl ether, combine the ether layers, wash with 30mL saturated NaCl aqueous solution until neutral, dehydrate through anhydrous sodium sulfate, concentrate in a water bath at 40±2°C to 0.3-0.5mL, blow dry with nitrogen, and dilute to 5.0 mL with acetone mL. After the sample liquid passes through a 0.45 μm filter membrane, it enters the gas chromatograph for determination, and the spectrum is shown in Figure 4 , record and contain propionic acid 0.42g / kg, dimethyl fumarate 0.075g / kg in this vinegar.

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Abstract

The invention relates to a detection method for determining a plurality of corrosion removers in food by gas chromatography. The target is that the method has the characteristics of simple operation, matrix interference resistance, reliable result and the like, and the method is suitable for accurately determining the content of the plurality of corrosion removers in the food. The technical scheme is that the gas chromatography detection method of the plurality of corrosion removers in the food is processed according to the following steps: 1) preparing sample extracting solution; preparing liquid sample extracting solution, or preparing solid sample extracting solution; 2) concentrating; rotatably concentrating the sample extracting solution in a water bath at 40+/-2 DEG C until the volume is 0.3-0.5mL; drying by nitrogen, and determining the volume to 2.0-5.0mL by acetone, filtering the sample solution by 0.45 micron of filter membrane to test; and 3) detecting on a machine: inputting the solution to be tested into a gas chromatograph with a hydrogen flame detector to detect.

Description

technical field [0001] The invention relates to a detection method, in particular to a detection method for gas chromatographic determination of various preservatives in food. Background technique [0002] Preservative refers to the agent that inhibits the corruption of substances, that is, it has a continuous inhibitory effect on the growth of microorganisms that use spoilage substances as metabolic substrates, and is widely used in food, daily chemical and other fields. [0003] There are many types of preservatives that are allowed to be added internationally, such as about 50 in the United States and 40 in Japan. At present, my country has only approved 32 kinds of food preservatives that are allowed to be used. They have undergone a lot of scientific experiments before being approved for use. They are all low-toxic and safe varieties, mainly including: benzoic acid and its sodium salt, Sorbic acid and its potassium salt, sulfur dioxide, sodium (potassium) metabisulfite,...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/06
Inventor 顾秀英许荣年鲍忠定欧菊芳杨琳王东铭王哲
Owner 浙江公正检验中心有限公司
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