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Method for measuring contents of coumarin and safrole in tobacco products

A technology for tobacco products and coumarin, which is applied in measuring devices, instruments, scientific instruments, etc., can solve the problems of time-consuming, labor-consuming, solvent-consuming, etc., and achieve the advantages of short analysis time, good chromatographic separation, and elimination of chromatographic interference. Effect

Active Publication Date: 2014-08-13
JILIN TOBACCO IND
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, these sample pretreatment methods have disadvantages such as time-consuming, labor-intensive, and solvent-consuming.

Method used

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  • Method for measuring contents of coumarin and safrole in tobacco products
  • Method for measuring contents of coumarin and safrole in tobacco products
  • Method for measuring contents of coumarin and safrole in tobacco products

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0087] Weigh 0.0500g of coumarin and 0.0500g of safrole standard respectively in a 100mL volumetric flask, dilute with dichloromethane to volume and shake well to obtain 500.0mg L -1 Mix the standard solution, as the standard stock solution I. Then dilute with dichloromethane to a concentration of 5 mg·L -1 , shake well, store in the refrigerator, and set aside to obtain the standard stock solution II.

[0088] Pipette 0.1mL, 0.2mL, 1mL, 2mL of mixed standard stock solution II and 0.1mL of mixed standard stock solution I, respectively, and place them in five 10mL volumetric flasks to obtain standard working solutions of five concentration levels. Dichloromethane to the mark, shake well. The concentrations of the five standard solutions are 0.05mg·L in turn -1 , 0.1mg·L -1 , 0.5mg·L -1 , 1mg·L -1 , 5mg·L -1 .

[0089] Will obtain standard solution and carry out gas chromatography-mass spectrometry, wherein the condition of gas chromatography determination is:

[0090] ...

Embodiment 2

[0094] Tobacco product samples were taken, and after freeze-drying, the water content was kept at about 5%. The sample was pulverized and sieved through a 200-mesh sieve, and the sieved sample powder was put into a brown sample bottle and refrigerated for testing;

[0095] Take 0.5 g of tobacco product sample powder, ultrasonically extract it with 15 mL of dichloromethane for 20 min, then pass the extract through a 0.45 μm organic filter membrane and concentrate to 100 μL. Take 20 μL of extract, fill it into the sample pool of ME-101 micro-extractor, seal the mouth of the sample pool with a septum, insert a 100 μL micro-syringe vertically into the sample pool through the condensing device, to a proper position under the septum, and insert it into the micro-syringe 10 μL of extraction solvent was added to start the extraction, and the extraction time was 4 min. The parameters of ME-101 multifunctional micro-extractor are:

[0096] The extraction conditions of air purging micr...

Embodiment 3

[0099] Using the method of Example 2, test the influence of extraction time on the extraction efficiency of coumarin and safrole. The difference is that in this example, the extraction temperature is 160°C, and the extraction time is 3min, 4min, and 5min respectively, and each experiment is done in parallel. three times.

[0100] The result is as image 3 as shown, image 3 The bar graph that the extraction time that the embodiment of the present invention 3 obtains influences on the extraction efficiency of coumarin and safrole, the result shows that when the extraction time is 3min, the average recovery rate of coumarin and safrole is 69% and 75%, and the RSD value is less than 15%; and when the extraction time is 4-5min, the average recovery rate of the target substance is 92%-114%, the relative standard deviation is less than 9.91%, and the recovery rate and precision meet the analysis requirements.

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Abstract

The invention provides a method for measuring the contents of coumarin and safrole in tobacco products. The method comprises the steps of carrying out ultrasonic extraction, filtering with an organic filter membrane and microextraction on the tobacco products to obtain a tobacco product solution to be measured; and performing gas chromatography-mass spectrometry detection on the tobacco product solution to be measured, thus obtaining the contents of coumarin and safrole in the tobacco products according to an acquired chromatogram of the tobacco product and preset standard curves of coumarin and safrole, so that the effect of simultaneously measuring coumarin and safrole in the tobacco products is achieved. The method can rapidly and accurately measure the contents of coumarin and safrole in the tobacco products, reduces the matrix effects and improves the separation degree of coumarin and safrole by adopting the microextraction technology; and the method has simplicity and convenience in operation.

Description

technical field [0001] The invention relates to the technical field of physical and chemical detection of tobacco products, in particular to a method for measuring the contents of coumarin and safrole in tobacco products. Background technique [0002] Coumarin, also known as o-hydroxycinnamic acid lactone and 1,2-benzopyrone, is a lactone compound that exists widely in nature, and it is the most abundant in Rutaceae and Umbelliferae. It also exists in other plants. Studies have reported that coumarin is a toxin precursor that will be converted into dicoumarin, and dicoumarin has an anticoagulant effect, which can cause capillary hemorrhage in animals and eventually damage the internal organs of animals. Safrole (safrole), also known as safrole and safrole, mainly exists in the essential oils of camphor plants such as submerged camphor and camphor, and is also used in the synthesis of spices such as jasmonal, vanillin and piperonyl butoxide. An important raw material and a ...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/08
Inventor 崔龙吉李东浩金玉善李光雄池敬姬李河霖赵锦花
Owner JILIN TOBACCO IND
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