CN101169398B

CN101169398B - Method for determining glyceryl triacetate in cigarette main flue

Info

Publication number: CN101169398B
Application number: CN2007101697889A
Authority: CN
Inventors: 朱立军; 戴亚
Original assignee: China Tobacco Chuanyu Industrial Co Ltd
Priority date: 2007-11-20
Filing date: 2007-11-20
Publication date: 2012-01-04
Anticipated expiration: 2027-11-20
Also published as: CN101169398A

Abstract

The invention relates to a method of measuring the triacetyl glycerine in the main smoke of cigarettes by a gas chromatogram method, in particular to a method of collecting and extracting the triacetyl glycerine in the main smoke of cigarettes. By use of the method, the cigarette sample has CV lower than 1.5 percent, and the recovery rate ranges from 98 percent to 100 percent; thus, the invention has the advantages of perfect repeatability and high recovery rate, thereby being applicable to analyzing the triacetyl glycerine in the main smoke of cigarettes.

Description

A kind of method of measuring triacetyl glycerine in the cigarette mainstream flue gas

Technical field

The present invention relates to the method for triacetyl glycerine in a kind of gas chromatography determination cigarette mainstream flue gas, particularly realize measuring the capture method and the extracting process of triacetyl glycerine in the cigarette mainstream flue gas.

Background technology

The plastifier of the fine mouth rod of triacetyl glycerine Chang Zuowei vinegar in tobacco processing process through adding triacetyl glycerine, can improve the physical indexs such as hardness of the fine mouth rod of vinegar.

Triacetyl glycerine has sizable amount directly to get into main flume when cigarette burns and sucks in the cigarette filter tip, is held back by cambridge filter as the flue gas granule phase substance, is one of tar main composition, accounts for about 5% of releasing content of coke tar usually, even more.Therefore, accurately measure the content of triacetyl glycerine in cigarette mainstream flue gas, the formation for understanding the cigarette mainstream flue gas tar content instructs the reasonable use of triacetyl glycerine in the production of cigarettes process and stable roll smoke product quality significant.

The domestic report that does not still have triacetyl glycerine method in the gas chromatography determination cigarette mainstream flue gas.The invention discloses the method for triacetyl glycerine in the exhibition gas chromatography determination cigarette mainstream flue gas.

Summary of the invention

The objective of the invention is to adopt the capture method of science and the accurate mensuration that extracting process is realized triacetyl glycerine in the cigarette mainstream flue gas.

The technical scheme that the present invention takes is:

1. cigarette sample is positioned in the environment of temperature (22 ± 1) ℃ and relative humidity (60 ± 2) % and regulates 48h, the cigarette after the adjusting props up and is specimen.

2. be with smoking machine suction specimen cigarette in the environment of (22 ± 2) ℃ and relative humidity (60 ± 5) % and under the standard aspiration condition in temperature; Capture the triacetyl glycerine in the cigarette mainstream flue gas with cambridge filter; Every kind of cigarette sample aspirates 2 groups, 20/group.

3. transfer in the 250mL conical flask capturing good cambridge filter, add 50mL and contain a certain amount of interior target isopropyl alcohol extract, oscillation extraction 2h.

4. with the triacetyl glycerine content in the gas chromatographic analysis isopropyl alcohol extract.

5. GC conditions: sample size 2 microlitres; 250 ℃ of injector temperatures, pressure (constant voltage) 110kPa, partial flow rate 15mL/min column oven: 110 ℃ (1min) 10 ℃/min150 ℃ (1min) 30 ℃/min230 ℃ (6min); Detecting device is FID, and temperature is 275 ℃, and hydrogen flowing quantity is 35mL/min, and air mass flow is 350mL/min, and the make-up gas? flow is 30mL/min; Chromatographic column is PE Elite-wax (crossbond-PEG) 30m * 0.25mmID * 0.25 μ mdf.

Concrete application examples 1

With isopropyl alcohol preparation (containing a certain amount of interior mark) extract; Prepare the triacetyl glycerine standard solution of 6 concentration gradients again with extract; Use the above-mentioned standard solution of gas chromatographic analysis then; By the working curve of internal standard method making triacetyl glycerine, obtain the correction equation (seeing table 1) of triacetyl glycerine.Visible by table 1, the correlativity of equation is good.

Table 1. triacetyl glycerine working curve drawing result

Standard specimen progression	Triacetyl glycerine (μ g/mL)	Peak area ratio
			1 2 3 4 5 6	34.927 69.854 139.701 209.563 279.418 349.272	0.0769 0.1522 0.2878 0.4381 0.5775 0.7164
Correction equation	Y＝2.03597E-03X+7.42648E-03
			R ²	0.9998

Annotate: E-03 representes 10 ^-3

Concrete application examples 2

By the said determination method triacetyl glycerine in certain trade mark cigarette sample flue gas is carried out 5 replicate determinations, result's (table 2) shows that its RSD is all less than 1.5%, and the repeatability of illustration method better.

Table 2 triacetyl glycerine repeatability is measured the result

Concrete application examples 3

Use the sample cigarette in the concrete application examples 2 to be laboratory sample; And in capturing good cambridge filter, add a certain amount of triacetyl glycerine standard solution; Press the said determination method and measure its content; The standard specimen amount of triacetyl glycerine actual content in the cigarette mainstream flue gas and adding is calculated the recovery of triacetyl glycerine respectively per sample, and the result sees table 3.This shows that the accuracy of method is higher.

Table 3. triacetyl glycerine determination of recovery rates result

Compound	Triacetyl glycerine
			1	2
	Sample size (μ g/mL) measured value (μ g/mL) measured value-sample size (μ g/mL) adds standard specimen amount (μ g/mL) recovery (%)	93.458 230.018 136.560 137.077 99.62			86.783 461.612 374.829 381.857 98.16
Recovery mean value (%)			98.89

Claims

1. a method of measuring triacetyl glycerine in the cigarette mainstream flue gas is characterized in that comprising the steps:

Step 1, cigarette sample is positioned in the environment of 22 ± 1 ℃ of temperature and relative humidity 60 ± 2% and regulates 48h, the cigarette after the adjusting props up and is specimen;

Step 2, be with smoking machine suction specimen cigarette in 22 ± 2 ℃ of environment with relative humidity 60 ± 5% and under the standard aspiration condition in temperature; Capture the triacetyl glycerine in the cigarette mainstream flue gas with cambridge filter; Every kind of cigarette sample aspirates 2 groups, 20/group;

Step 3, transfer in the 250mL conical flask capturing good cambridge filter, add 50mL contain a certain amount of in target isopropyl alcohol extract, oscillation extraction 2h;

Step 4, with the triacetyl glycerine content in the gas chromatographic analysis isopropyl alcohol extract;

The GC conditions of step 4 wherein: sample size 2 microlitres; 250 ℃ of injector temperatures, pressure 110kPa, partial flow rate 15mL/min; Column oven: initial temperature keeps 1min for 110 ℃, rises to 150 ℃ with 10 ℃/min, keeps 1min, rises to 230 ℃ with 30 ℃/min, keeps 6min; Detecting device is FID, and temperature is 275 ℃, and hydrogen flowing quantity is 35mL/min, and air mass flow is 350mL/min, and the make-up gas? flow is 30mL/min; Chromatographic column is PE Elite-wax 30m * 0.25mmID * 0.25 μ mdf.