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Internal standard method based quantifying method for thermal cracking product of additives for tobacco

A pyrolysis product and thermal cracking technology, applied in measuring devices, instruments, scientific instruments, etc., can solve the problem of unreported quantitative analysis of cracked products, and achieve the effects of unlimited physical state of the sample, good reproducibility, and accurate quantification.

Active Publication Date: 2012-08-15
ZHENGZHOU TOBACCO RES INST OF CNTC
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] Literature research shows that the above studies on pyrolysis products are all focused on qualitative analysis, and the quantitative analysis of pyrolysis products has not been reported yet

Method used

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  • Internal standard method based quantifying method for thermal cracking product of additives for tobacco
  • Internal standard method based quantifying method for thermal cracking product of additives for tobacco

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] 1. Prepare a certain absolute oil solution with a concentration of about 10 mg / ml, inject 2 ul sample into the middle section of the pyrolysis tube of the probe of the pyrolysis instrument and fill it with quartz wool to fix it; use CDS PYROPROBE2000 thermal pyrolysis instrument for pyrolysis, and the control conditions in the process are: The initial temperature of the pyrolysis instrument probe: 50°C; the heating rate: 20°C / millisecond; the final temperature rises to 400°C and 800°C respectively, the pyrolysis time is 10s, and the volume percentage of oxygen in the pyrolysis atmosphere is 20%; The GC analysis conditions for MS to separate and detect pyrolysis products are as follows: Injection port temperature: 250°C; carrier gas: He, flow rate 0.8ml / min, chromatographic column: HP-FFAP column (30m×0.25mm×0.25μm) ; split ratio 20:1; hold for 20min; GC / MS temperature program: initial temperature 40°C, final temperature 220°C, heating rate 5°C / min; mass spectrometry cond...

Embodiment 2

[0035]1. Weigh 0.1 mg of a natural polysaccharide extract (self-made, colorless and odorless white solid powder at room temperature, purity >99%), put it into the middle section of the cracking tube of the CDS PYROPROBE2000 cracking instrument probe and fill it with quartz wool to fix the sample. Carry out pyrolysis experiments: the initial temperature of the pyrolysis instrument probe: 100°C; the heating rate: 10°C / millisecond; the final temperature rises to 300, 600, and 900°C respectively, the pyrolysis time is 5s, and the volume percentage of oxygen in the pyrolysis atmosphere is 0%; GC analysis conditions for the separation and detection of pyrolysis products by using GC-MS coupled with a pyrolyzer are as follows: inlet temperature: 270°C; carrier gas: He, flow rate 1.2ml / min, chromatographic column HP-5MS (60m×0.25mm.×0.25μm), split ratio 50:1; hold for 40min; GC / MS temperature program: initial temperature 50℃, final temperature 270℃, heating rate 2℃ / mi; The mass spectro...

Embodiment 3

[0044] 1. Prepare a monomer fragrance solution with a concentration of 17 mg / ml, inject 1 μl of the sample into the middle section of the cracking tube of the pyrolysis instrument probe and fill it with quartz wool; put it into the middle section of the cracking tube of the CDS PYROPROBE2000 cracking instrument probe and fill it with quartz wool. Carry out pyrolysis experiment on the sample: the initial temperature of the pyrolysis instrument probe: 60°C; the heating rate: 30°C / millisecond; the final temperature rises to 600 and 900°C respectively, the pyrolysis time is 3s, and the volume percentage of oxygen in the pyrolysis atmosphere is 20%; the GC analysis conditions for separation and detection of pyrolysis products by using GC-MS coupled with a pyrolyzer are as follows: inlet temperature: 270°C; carrier gas: He, flow rate 1.0ml / min, chromatographic column u2 (5m ×0.25mm.×0.25μm), split ratio 100:1; hold for 10min; GC / MS temperature program: initial temperature 40℃, final ...

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Abstract

The invention discloses an internal standard method based quantifying method for a thermal cracking product of additives for tobacco. The method is characterized in that a sample is pre-cracked by a gas chromatograph, a mass spectrograph and conditions, thermal cracking product is separated to be detected, and the thermal cracking product is retrieved and determined according to retention time and a mass spectrum database; then, an internal standard substance is selected and prepared into the internal standard solution with certain concentration, and the cracking product ingredient to be quantified is prepared into the standard solution with certain concentration; in a cracking tube, the equivalent internal standard solution is respectively added into the sample to be cracked and the standard solutions with different concentrations to carry out cracking and separating detection; the cracking product and the internal standard substance are determined according to the retention time andthe mass spectrum database; and a standard curve is drawn according to the ratio of the cracking product peak area to the internal standard substance peak area so as to quantify the cracking product.The method has the advantages of accurate quantification for thermal cracking product of additives for tobacco, good reproducibility, large information amount, no limit to physical state and the like.

Description

[0001] technical field [0002] The invention belongs to the field of tobacco chemistry, and specifically relates to a method for quantifying pyrolysis products of tobacco additives based on an internal standard method. The pyrolysis product is determined by cracking the target substance, and then the internal standard and different concentrations of the pyrolysis product components are tested under the same conditions. The pyrolysis was carried out under the following conditions, and the standard curve was established by the ratio of the peak area of ​​the pyrolysis product to the peak area of ​​the internal standard, so as to quantify the pyrolysis product of the tobacco additive. [0003] Background technique [0004] Cigarettes are a special hobby product, and smoking is to obtain certain satisfaction by smoking the smoke produced by burning cigarettes. The components of cigarette smoke are formed through complex processes such as combustion, cracking, degradation, a...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/06
Inventor 宋瑜冰李炎强宗永立李鹏卢斌斌孙世豪杨春强蒋成勇
Owner ZHENGZHOU TOBACCO RES INST OF CNTC
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