A kind of assay method of menthol in essence and spices for tobacco

A technology of tobacco flavor and determination method, which is applied in the field of chemical analysis and detection, can solve the problems of affecting work efficiency, low determination result, long operation time, etc., and achieves the effects of improving measurement accuracy, extraction accuracy and good repeatability

Active Publication Date: 2016-11-16
CHINA TOBACCO SHAANXI IND
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  • Abstract
  • Description
  • Claims
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Problems solved by technology

[0004] The disadvantage of Yang Hong's menthol determination method is that during the sample pretreatment process, anhydrous sodium sulfate is added, left overnight, and filtered with qualitative filter paper, because anhydrous sodium sulfate and filter paper are adsorptive, which may lead to low measurement results. If placed overnight, the operation time is too long, which affects work efficiency; on the other hand, the quantitative method adopts the external standard method, which is not as accurate as the internal standard method.

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  • A kind of assay method of menthol in essence and spices for tobacco
  • A kind of assay method of menthol in essence and spices for tobacco
  • A kind of assay method of menthol in essence and spices for tobacco

Examples

Experimental program
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Effect test

Embodiment 1

[0045] Embodiment 1: the selection of extraction solvent

[0046] In this example, four organic solvents, n-hexane, dichloromethane, n-pentane, and ethyl acetate were selected as extraction solvents to extract menthol in flavors and fragrances respectively, and 0.3g of tobacco flavors and fragrances were taken in 50mL Mokou Triangle Add 10mL of the four extracts containing the internal standard concentration of 180μg / mL to the bottle, shake and extract for 30min, take the supernatant, analyze according to the GC-MS conditions in step 1.4, and calculate the The content of menthol in flavors and fragrances; the experimental results show that there are more propylene glycol solvent extractions in the samples extracted by dichloromethane and ethyl acetate, and the separation of propylene glycol peaks and menthol peaks is not good, which is not conducive to the analysis of menthol. The extraction of the solvent propylene glycol by alkanes is relatively low, because the properties o...

Embodiment 2

[0049] Embodiment 2: the selection of extraction method

[0050] In order to investigate the influence of the extraction method on the extraction effect, the experiment of this example compares the two extraction methods of ultrasonic extraction and vibration extraction. Take 1.0 g of tobacco flavor and fragrance in a 50 mL ground-mouth conical flask, and add an internal standard with a concentration of 180 μg 15mL of n-hexane extract per mL, ultrasonic and vibration extraction respectively after 40min, get the supernatant, analyze by the GC-MS condition in step 1.4, and calculate the content of menthol in the essence and spices for tobacco; Result It shows that the water temperature in the ultrasonic extraction process will increase with the extraction time, and the components in the essence are mainly volatile components, which affect the analysis results, so the extraction method is chosen as vibration extraction.

[0051] Table 3 Comparison of menthol extraction results by...

Embodiment 3

[0053] Embodiment 3: the selection of extraction volume

[0054] This example investigates the situation of different extraction volumes on the extraction efficiency of menthol. Add 2, 5, 10, 15, 20, 25, 30, 35, and 40 mL of different volumes to contain the internal standard concentration of 180 μg / mL n-hexane extract, shake and extract for 50min, take the supernatant respectively, analyze according to the GC-MS conditions in step 1.4, and calculate the content of menthol in the flavor and fragrance for tobacco; the results are shown in Table 4 Shown, show that the extraction rate of menthol increases with the increase of extraction volume before 5mL, and decreases with the increase of extraction volume after 5mL, so extraction volume selection is 2~15mL among the present invention, optimal extraction volume selection is 5mL.

[0055] Table 4 Comparison of different extraction volumes on menthol extraction efficiency

[0056]

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Abstract

The invention relates to a method for determining menthol in tobacco flavor and perfume. The method comprises the following steps: adding N-hexane extraction liquid containing an internal standard into the tobacco flavor and perfume, and thus obtaining a sample solution; after oscillation extraction, getting supernatant for GC-MS analysis, and thus obtaining the peak area ratio of menthol and the internal standard in the sample supernatant; preparing a menthol-series standard work-solution by using menthol and the N-hexane extraction liquid containing the internal standard for GC-MS analysis, and thus obtaining the peak area ratio of menthol to the internal standard in the standard work-solution; establishing an equation of linear regression through the peak area ratio of menthol to the internal standard in the standard work-solution and the mass concentration of menthol, obtaining the mass concentration of menthol in the standard work-solution, and calculating the content of menthol in the tobacco flavor and perfume. The method adopts a solvent for direct extraction, an internal standard method for quantification and a GC-MS method for the determination of menthol content, so that the accuracy of determination of menthol in the flavor and perfume and the working efficiency are improved, and meanwhile the menthol loss in the experimental process is reduced.

Description

technical field [0001] The invention belongs to the technical field of chemical analysis and detection, and in particular relates to a method for determining menthol in flavors and fragrances for tobacco. Background technique [0002] Menthol is a commonly used cigarette cooling additive. Adding an appropriate amount of menthol to cigarettes can ease the irritation of smoke and remove green miscellaneous gases. See Zhong Qinghui. A brief discussion on the application of cigarette flavoring technology[J]. Tobacco Science, 1996, (4): 30. Menthol in tobacco is mainly used in cigarette filter rods, cigarette paper, cigarette shreds, tobacco sheets, etc. It is mainly added in the way of flavors and fragrances to achieve the goal of improving cigarette smoke. Therefore, the determination of mint in cigarette flavors and fragrances Alcohol is of great significance for improving the quality stability of cigarette products. [0003] Because of its cool and special properties, menth...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/02
Inventor 樊亚玲黄仲波李春王大锋曹洁穹彭军仓何育萍吕娟杨芳徐磊
Owner CHINA TOBACCO SHAANXI IND
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