Method for analyzing residual solvent in explodable bead of cigarette filter based on HS-GC (head space-gas chromatography)/MS (mass spectrometry) technology

A technology for cigarette filter tip and technical analysis, which is applied in the field of analyzing solvent residues in cigarette filter tip popped beads based on HS-GC/MS technology, and achieves the effects of simple pretreatment process, accurate measurement results and low cost

Inactive Publication Date: 2017-05-31
CHINA NAT TOBACCO QUALITY SUPERVISION & TEST CENT
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

How to detect the amount of solvent residue in cigarette filter popping beads (wall material and core material) has not been reported so far

Method used

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  • Method for analyzing residual solvent in explodable bead of cigarette filter based on HS-GC (head space-gas chromatography)/MS (mass spectrometry) technology
  • Method for analyzing residual solvent in explodable bead of cigarette filter based on HS-GC (head space-gas chromatography)/MS (mass spectrometry) technology
  • Method for analyzing residual solvent in explodable bead of cigarette filter based on HS-GC (head space-gas chromatography)/MS (mass spectrometry) technology

Examples

Experimental program
Comparison scheme
Effect test

example 1

[0035]Cigarette filter popping beads are a kind of circular capsule with fragrance added to the filter rod for cigarettes, which can release fragrance when subjected to a certain external force. In order to detect the solvent residue in the popping beads of cigarette filters, it is first necessary to break the wall of the popping beads. The experimental results show that the wall material of cigarette filter popping beads cannot be dissolved by common organic solvents. If the wall is broken by means of ultrasound and vibration for a long time, it will easily cause the loss of volatile target analytes. If only the popping beads are soaked It is not conducive to the complete dissolution of the solvent residue in the explosive beads if the sample is loaded for analysis after breaking. Therefore, it is a better sample pretreatment method to crush the explosive beads in a short time by external force. In order to avoid the loss caused by the residue of the explosive beads in the co...

example 2

[0038] According to the configuration standard working solution method that the inventive method recommends, then according to the instrument condition of the inventive method, get 5 grade series standard working solutions and carry out HS-GC / MS analysis, with the response peak area ratio of solvent residual concentration and solvent residual and internal standard Draw standard curve and standard working curve regression equation (see Figure 4 , 5 ). The limit of detection (LOD) was calculated at 3 times the signal-to-noise ratio (S / N = 3), and the limit of quantification (LOQ) was calculated at 10 times the signal-to-noise ratio (S / N = 10), while considering the possibility of recovery results Acceptability, detection limit and limit of quantitation of the final obtained method are shown in Table 2.

[0039]

example 3

[0041] Using typical detection samples (such as Image 6 ), the recovery and precision experiments were carried out with the 3-level standard addition method, and the determination was repeated 5 times for each standard addition level. The recovery and repeatability results of the detection method are shown in Table 3. It can be seen from Table 3 that the recovery rate and repeatability data are ideal, the recovery rates of the three spiked levels are between 79.1-112.0%, and the relative standard deviation (RSD) is 0.5-14.9%, which can meet the needs of quantitative analysis.

[0042]

[0043] .

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Abstract

The invention discloses a method for analyzing a residual solvent in an explodable bead of a cigarette filter based on the HS-GC (head space-gas chromatography) / MS (mass spectrometry) technology. The method is characterized in that after a sample is pinched to be broken by an external force, a matrix correction agent and an internal standard into a head space bottle, a cover is applied for sealing, and the HS-GC / MS method is used for measuring the residual solvent in the explodable bead of the cigarette filter under certain equilibrium temperature and certain equilibrium time. According to the method, unknown ingredients contained in the sample can be monitored while the residual solvent in the explodable bead of the cigarette filter is simply and quickly detected. The universality is wide, the expandability is strong, the detection result is accurate, the repeatability is good, the pre-treating process is simple, and easy operation, high throughout and low cost are realized.

Description

technical field [0001] The invention belongs to the technical field of chemical analysis, and mainly relates to a method for analyzing solvent residues in cigarette filter popping beads based on HS-GC / MS technology, that is, benzene, toluene, ethylbenzene, (o-, m-) in cigarette filter popping beads. , p)xylene, styrene, methanol, ethanol, isopropanol, n-propanol, n-butanol, acetone, 4-methyl-2-pentanone, butanone, cyclohexanone, ethyl acetate, n-acetate Propyl ester, n-butyl acetate, isopropyl acetate, 2-ethoxyethyl acetate, 1-methoxy-2-propanol, 1-ethoxy-2-propanol, 2-ethoxy Headspace-Gas Chromatography / Mass Spectrometry Test Method for Solvent Residues in Ethanol, Dimethyl Succinate, Dimethyl Glutarate, and Dimethyl Adipate. Background technique [0002] Solvent residues in smoking materials are basically brought by the raw materials themselves and chemicals such as binders used in post-processing. Solvents) will cause carcinogenic, teratogenic, mutagenic and other hazar...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/06
CPCG01N30/02G01N30/06G01N2030/045
Inventor 刘珊珊刘岩顺范子彦王颖李中皓边照阳杨飞邓惠敏唐纲岭
Owner CHINA NAT TOBACCO QUALITY SUPERVISION & TEST CENT
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