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Method for determining menthol in cigarette filter rod

A technology for cigarette filter rods and determination methods, which is applied in the field of chemical analysis, can solve the problems of rare reports of samples, long analysis time, and no separation ability, etc., and achieve the effects of wide application range, good repeatability, and strong practicability

Active Publication Date: 2012-02-15
CHINA TOBACCO ZHEJIANG IND
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] Among the existing methods, regardless of colorimetry, near-infrared spectroscopy, conductometric titration, and optical rotation, these methods have no separation ability, and there must be no interfering substances in the analysis. The analysis time is long and the efficiency is low.
Therefore, gas chromatography is the most commonly used method for menthol detection, and gas chromatography mainly contains capillary column method, packed column method (packed column separation effect is not as good as capillary column) and 14C labeling method (mainly used for the chiral structure of menthol analysis), but the method for the determination of menthol in cigarette filter rods is rarely reported due to the complexity of the sample

Method used

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  • Method for determining menthol in cigarette filter rod
  • Method for determining menthol in cigarette filter rod
  • Method for determining menthol in cigarette filter rod

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0050] 1 Materials and methods

[0051] 1.1 Reagents and instruments

[0052] (-)-menthol, purity greater than 99%; n-propyl benzoate, purity greater than 99%; absolute ethanol, domestic analytical grade; rotary oscillator (THZ-320); analytical balance, Mettle, sensitivity 0.1mg; Agilent6890 gas chromatograph, equipped with flame ionization detector (FID), autosampler; HP-Innowax fused silica capillary column (30m×0.25mm×0.25μm); filter, agilent, aqueous or organic phase, 0.45um ; Disposable sterile syringe: 2ml; pipette gun (100ul-1000ul); other common experimental glassware.

[0053] 1.2 Experimental samples (test within 1 month):

[0054] Fragrant thread mint filter stick refers to the peppermint filter stick prepared by fragrant thread method in the art, referred to as fragrant thread mint filter stick.

[0055] There are three kinds of specifications of domestic incense mint filter sticks: domestic incense mint filter stick I (menthol content 10mg / stick), domestic ince...

Embodiment 2

[0121] Determination of the number of samples:

[0122] According to GB / T 5605 "Fiber Acetate Filter Sticks of Tobacco and Tobacco Products" Part 6 (Inspection Rules), 1,000 mint filter sticks (Zhejiang China Tobacco Mint Filter Sticks) were taken as laboratory samples for the sample quantity determination test. Randomly extract 2, 3, 5 and 10 samples from the laboratory samples for uniformity test, 30 times in total. The test results and mathematical statistics are as follows;

[0123] Table 7 The menthol content of a single stick tested with different counts

[0124]

[0125]

[0126] From the coefficient of variation and range analysis in Table 7, it is shown that the order of the dispersion of the test results is 2, 3, 5, and 10. As the number of samples increases, the experimental results tend to be stable.

[0127] The 30 groups of data in Table 7 are evaluated for normality of data, and the normal probability map is as follows Figure 4 As shown, under the cond...

Embodiment 3

[0142] Loss of Menthol in Cigarette Filter Rod

[0143] Menthol will sublime in the air, in order to ensure the stability of the test data, it should be stored in -4°C refrigerator, room temperature, constant temperature and humidity: temperature (22±2)°C and humidity (60±5)RH%. The same brand and the same batch of cigarette filter sticks (Zhejiang China Tobacco Mint Filter Stick) under different storage conditions have been measured, and the assay method is the same as the analytical test method in Example 1, and the results are as follows Figure 5 shown.

[0144] From Figure 5 It can be seen that the menthol content of the filter sticks decreased slowly under the storage condition of -4°C, and the content decreased significantly under the other two conditions. Therefore, when the filter stick sample is at room temperature or in a state of constant temperature and humidity, the experiment must be carried out as soon as possible. It is recommended that the laboratory samp...

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Abstract

The invention discloses a method for determining menthol in a cigarette filter rod, comprising the flowing steps of: extracting the cigarette filter rod by the use of an extractant to obtain an extraction solution; dissolving menthol by the use of the extractant, followed by a constant volume process, preparing a standard storing solution, and diluting the standard storing solution by the use of the extractant to obtain working standard liquids at a series of concentrations; respectively carrying out chromatography on the working standard liquids and the extraction solution under the same condition by the FID-capillary column gas chromatography method to obtain a chromatogram; calculating the peak area ratio of menthol to an internal standard substance in each working standard liquid, andmaking out the linear regression equation of the menthol concentration and the peak area ratio; calculating the peak area ratio of menthol to the internal standard substance in the extraction solution, and calculating the concentration of menthol in the extraction solution according to the linear regression equation; and calculating the content of menthol in the cigarette filter rod. The method provided by the invention is stable and accurate, is simple to operate, has strong practicality, good repeatability and a wide application range, and can be used for the determination of menthol in filter rods within the industry.

Description

technical field [0001] The invention relates to the field of chemical analysis, in particular to a method for determining menthol in cigarette filter sticks. Background technique [0002] Mint spices include peppermint oil and spearmint oil, which is the third largest type of spice in the world, and the main aroma substance is menthol. Menthol, also known as menthol, hexahydrothymol, chemical name 1-methyl-4-isopropylcyclohexan-3-ol, molecular formula C 10 h 20 O, melting point 42-43°C, boiling point 212°C, density 0.890g / cm 3 , colorless columnar or needle-like crystals at room temperature, sublimation when exposed to air, slightly soluble in water, miscible with ethanol and propylene glycol (Wang Zhen; Chemical Dictionary [M]; Beijing: Chemical Industry Press, 1987( Second edition): 728~729.), its structural formula is as follows: [0003] [0004] Menthol has 4 pairs of isomers, each of which has left-handed, right-handed and racemic forms, and their aroma properti...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/06G01N30/86
Inventor 张卫平陆明华王雨凝朱书秀夏骏张云莲
Owner CHINA TOBACCO ZHEJIANG IND
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