Silylation GC/MS (gas chromatography-mass spectrometry) detection method for simultaneous determination of saccharide, 1, 2-propylene glycol and glycerin in tobacco

A detection method, the technology of propylene glycol, applied in the direction of measuring devices, instruments, scientific instruments, etc., can solve the problems of high detection limit and inaccurate characterization, and achieve the effect of high sensitivity, strong specificity and simple pretreatment

Active Publication Date: 2015-04-29
CHINA TOBACCO GUANGDONG IND
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, this method has certain limitations. It is only qualitative by retention time, which is not accurate enough, and the detection limit of the method is usually high.
[0004] At present, there are no other relevant technical reports on the simultaneous determination of sugars such as glycerin, propylene glycol, fructose, glucose and sucrose in tobacco

Method used

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  • Silylation GC/MS (gas chromatography-mass spectrometry) detection method for simultaneous determination of saccharide, 1, 2-propylene glycol and glycerin in tobacco
  • Silylation GC/MS (gas chromatography-mass spectrometry) detection method for simultaneous determination of saccharide, 1, 2-propylene glycol and glycerin in tobacco
  • Silylation GC/MS (gas chromatography-mass spectrometry) detection method for simultaneous determination of saccharide, 1, 2-propylene glycol and glycerin in tobacco

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0042] 1. Instrument

[0043] Agilent 6890 / 5973 GC / MS, Agilent 7683 autosampler (Agilent, USA); chromatographic column: DB-5 MS column, the specification is 60m×0.25mm×0.25μm.

[0044] 2. Reagents

[0045] N,O-bis(methyl)trifluoroacetamide (BSTFA) (Regis Technologies, USA); N,N-dimethylformamide (DMF) (CNW Technologies GmbH, Germany); phenylethyl acetate-D3 ( Internal standard) (purity 98%, CDN isotopes, Canada); 1,2-propanediol, glycerol, fructose, glucose, sucrose (Sigma-Aldrich, Germany).

[0046] 3. Solution preparation

[0047] Preparation of internal standard solution: Accurately weigh about 500mg of phenylethyl acetate-D3 into a 50mL volumetric flask, dilute to the mark with dichloromethane, this solution is the internal standard solution of phenylethyl acetate-D3

[0048] Preparation of extraction solution: Accurately pipette 2.00mL of phenylethyl acetate-D3 internal standard stock solution into a 100mL volumetric flask, and dilute to the mark with DMF and BSTFA sol...

Embodiment 2

[0099] The repeatability experiment of embodiment 2 inventive method

[0100] Apply the method of the present invention (with reference to the best detection conditions and detection steps determined in Example 1) to carry out repeatability test on the same flue-cured tobacco type cigarette, each sample is tested 5 times, and the relative standard deviation of the calculation method is calculated. The results are shown in Table 2, and the relative standard deviation of the measurement results is between 0.7% and 11.1%.

[0101] Table 2 Sample repeatability test results (unit mg / g)

[0102] target compound 1 2 3 4 5 average value RSD(%) 1,2-propanediol 3.76 3.7 3.6 3.21 3.22 3.50 7.6 glycerin 1.14 1.11 1.07 0.99 1.01 1.06 6.0 fructose 45.58 47.49 46.59 46.31 46.11 46.42 1.5 glucose 35.81 35.6 32.47 35.67 35.36 34.98 4.0 sucrose 8.42 8.66 8.02 8.00 8.20 8.26 3.4

Embodiment 3

[0103] The recovery rate of standard addition of embodiment 3 inventive method

[0104]Accurately weigh the same tobacco sample, measure its 1,2-propanediol, glycerol, fructose, glucose and sucrose concentrations with reference to the optimal detection conditions and detection steps determined in Example 1, and add three levels of high, medium and low respectively precisely Standard substance, each level parallel triplicate, prepare the test solution according to the method in section 1.5 and analyze and measure, calculate the recovery rate and relative standard deviation of the method, the results are shown in Table 3. The results showed that the recoveries of 1,2-propanediol, glycerol, fructose, glucose and sucrose ranged from 90.3% to 114.4%, with RSDs ranging from 0.4% to 9.1%, indicating that the method had good recoveries.

[0105] Table 3 The recovery rate of target substances in tobacco samples

[0106]

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Abstract

The invention discloses a silylation GC / MS (gas chromatography-mass spectrometry) detection method for simultaneous determination of saccharide, 1, 2-propylene glycol and glycerin in tobacco. A sample adopts DMF (dimethyl formamide) and BSTFA (N,O-bis(trimethylsilyl)trifluoroacetamide) as the extraction solvent and the derivatization reagent and has a derivatization reaction for 30 min in an oven at the temperature of 70 DEG C, DB-5MS chromatographic column with the size of 60m*0.25mm*0.25 mu m is adopted, and the content of 1, 2-propylene glycol, glycerin, fructose, glucose and sucrose is analyzed and determined with the GC / MS. Results show that the method has good linearity, the detection limit is 0.04-2.85 mg / g, the limit of quantitation is 0.13-9.61 mg / g, the average recovery of standard addition is 90.3%-114.4%, and the relative standard deviation is smaller than 9.1%. The use quantity of the sample and the reagent is small, the pretreatment is simple, and the method has the characteristics of fastness, simplicity, convenience, high sensitivity, high specificity and the like and is suitable for simultaneous determination of polyol compound and saccharide in a tobacco sample.

Description

technical field [0001] The invention relates to the technical field of tobacco detection, in particular to a silanized GC / MS detection method for simultaneously determining sugar, 1,2-propanediol and glycerin in tobacco. Background technique [0002] Humectants and sugars are commonly used additives in tobacco production. Polyol compounds such as propylene glycol and glycerin can maintain the moisture in tobacco, avoid the taste loss caused by moisture volatilization during cigarette storage, reduce roughness during processing, and have the functions of fixing fragrance and moisturizing, and are commonly used humectants , is widely used in tobacco, and its content in shredded tobacco of cigarettes can reach about 5%. Glucose, fructose and other sugars are important components in tobacco and tobacco feed liquid. They can play the role of bonding, adding ingredients, flavoring, acid production and moisturizing in tobacco products, especially in giving cigarettes aroma and Co...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/06
Inventor 赖燕华王华陈森林
Owner CHINA TOBACCO GUANGDONG IND
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