Method for measuring residual volatile components in cigarette filter stick

A technology of volatile components and filter rods, which is applied in the field of detection of 12 kinds of volatile components residues in cigarette filter rods, can solve the problems of unsuitable filter rod detection, cumbersome and repetitive operations, affecting the quality of smoke, etc., and achieves strong practicality. The effect of high price, good selectivity and high recovery rate

Active Publication Date: 2014-01-15
CHINA TOBACCO FUJIAN IND
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The cigarette filter rod is the part of the cigarette that is in direct contact with the mouth, which can filter the smoke, but at the same time, the residual volatile harmful components will also directly enter the lungs through smoking, which will directly cause harm to human health; and, During the cigarette smoking process, the temperature at the end of the filter rod can reach up to 80°C, and the volatile components contained in the cigarette filter rod will be distilled out and enter the mainstream smoke, thereby affecting the quality of the smoke
[0004] At present, the research on filter rods in the industry is concentrated on its application, but there are few researches on its own volatile component residues. The recent related reports include: Zhang Yingxin, Fan Yaling, Qin Hong published in the Journal of Mass Spectrometry in 2007, entitled The article "Solid Phase Microextraction-Gas Chromatography-Mass Spectrometry Rapid Analysis of Volatile Components of Propylene Filter Rod Adhesive"; Li Zhonghao, Tang Gangling, Chen Zaigen, etc., the title of the invention is "A Kind of Volatile Organic Compounds in Cigarette Filters" Determination method" patent application (CN102128906A), the study uses saturated sodium chloride aqueous solution as the matrix calibrator, fluorobenzene as the internal standard, and headspace-gas chromatography as the detection method to measure volatile organic compounds in cigarette filters, but due to alcohol Solubilities in sodium chloride aqueous solution are relatively large, therefore, this method is not applicable to the mensuration of methanol and other alcohols content, and, this method adopts Supelco VOCOL column, is a kind of medium polarity column, a large amount of in the sample to be tested The moisture in the medium polarity column (VOC column) will have a great destructive effect, which will easily lead to the failure of the column; Kong Haohui, Chen Cuiling, He Yanming, the title of the invention is "A Quantitative Detection Method for Volatile Organic Compounds in Cigarette Filter Stick Additives" Patent application (CN101650280A), using glycerol triacetate as solvent, using headspace-GC qualitative and headspace-gas chromatography quantitative, the combination of the two methods to detect volatile organic compounds in cigarette filter rod additives, operation Relatively repetitive and cumbersome, and the plasticizer of the filter rod is glycerol triacetate, therefore, this solvent is not suitable for the detection of filter rods

Method used

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  • Method for measuring residual volatile components in cigarette filter stick
  • Method for measuring residual volatile components in cigarette filter stick
  • Method for measuring residual volatile components in cigarette filter stick

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0061] 1. Instruments and reagents:

[0062] PerkinElmer TurboMatrix HS-40 headspace sampler, PerkinElmer Clarus600 gas chromatograph, PerkinElmer Clarus600MS detector, METTLER TOLEDO BT224S (sensitivity 0.1mg), 20ml headspace bottle, piston pipette, 1000μL.

[0063] Standard compounds: benzene, toluene, methanol, ethanol, isopropanol, acetone, methyl acetate, vinyl acetate, ethyl acetate, n-propyl acetate, n-butyl acetate, 1-methoxy-2-propanol, All are analytically pure.

[0064] Solvent (matrix calibrator): N,N-dimethylformamide; internal standard: fluorobenzene, all analytically pure.

[0065] Sample: filter rod for cigarettes.

[0066] 2. Standard solution preparation:

[0067] Weigh 0.0259 g of the internal standard fluorobenzene, dissolve it in 1 L of N,N-dimethylformamide solution, and configure the N,N-dimethylformamide solution containing the internal standard. Then weigh 0.0104g and 0.0385g each of benzene and toluene, and 0.2571g, 0.2358g, 0.2505g, and 0.2417g e...

Embodiment 2

[0090] According to the method and steps described in Example 1, six kinds of tobacco filter stick samples of A, B, C, D, E, and F are selected for measurement and analysis, and the specific results are shown in Table 5:

[0091] Table 5 Detection results of volatile components in cigarette filter sticks

[0092]

[0093] Note: " / " means not checked out.

Embodiment 3

[0094] Embodiment 3: detection limit and recovery rate contrast

[0095] The comparative analysis of the method of the present invention and Li Zhonghao et al.'s "A Determination Method for Volatile Organic Compounds in Cigarette Filters" (comparative method) in the three aspects of detection limit, recovery rate and coefficient of variation, the results are shown in Table 6 and Table 7.

[0096] Standard curve and detection limit of volatile components in table 6 cigarette filter stick

[0097]

[0098] Table 7 Repeatability and recovery rate of detection method for volatile component residues in cigarette filter sticks

[0099]

[0100]

[0101] As can be seen from Table 6 and Table 7, the common target compounds of the two methods are vinyl acetate, ethyl acetate, benzene, n-propyl acetate, toluene, and n-butyl acetate. For the 6 kinds of common targets, compared with the comparative method of Li Zhonghao et al., the quantitative detection limit of the present in...

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Abstract

The invention provides a method for measuring residual volatile components in a cigarette filter stick. The method is a headspace-gas chromatography/mass spectrum combined method and adopts an internal standard method to quantify, wherein in the headspace sampling process, N,N-dimethylformamide is used as a substrate correction agent. The method adopts a headspace sampling pretreatment mode, not only is convenient and rapid, but also can reduce loss of a sample due to complex pretreatment; the internal standard gas/mass combined method is adopted for measuring, misjudgment caused by false positive which possibly occurs to a complex system compound is avoided, influence of chromatographic conditions on a quantifying result is reduced and both accuracy and precision are relatively high. The method is used for measuring the volatile components in the cigarette filter stick, is simple, convenient, accurate and rapid to operate, and has good selectivity and strong practical value.

Description

technical field [0001] The invention belongs to the technical field of chemical detection of cigarette filter rod materials, and in particular relates to the detection technology of 12 kinds of volatile components remaining in the cigarette filter rod. Background technique [0002] With the increasing emphasis on cigarette safety by the National Administration, there are more and more types of safety index control for cigarette auxiliary materials and tobacco additives. In recent years, the national bureau has continuously carried out the determination and limit standards of safety and health indicators related to tobacco materials. The tobacco materials involved include trademark paper for cigarettes, lining paper, tipping paper, water-based glue, tow filter rods, etc. There are dozens of control indicators included (formaldehyde, methanol, ethanol, n-propanol, isopropanol, n-butanol, acetone, butanone, 4-methyl-2-pentanone, cyclohexanone, propylene glycol methyl ether, Pr...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/88
Inventor 黄惠贞梁晖刘秀彩张建平余玉梅林艳黄华发叶仲力张鼎方方钲中谢卫许寒春
Owner CHINA TOBACCO FUJIAN IND
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