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A method for determining the content of glyceryl monoacetate and glyceryl diacetate in triacetin for cigarettes

A technology of glycerol diacetate and glycerol acetate is applied in the field of determination of the content of glycerol monoacetate and glycerol diacetate in triacetin for cigarettes, and can solve problems affecting quantitative accuracy, acid return, and unqualified product quality. and other problems, to achieve the effect of simultaneous detection and accurate quantification, and accurate analysis and detection results

Active Publication Date: 2020-07-10
HUBEI CHINA TOBACCO IND
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Glyceryl triacetate will undergo saponification reaction (that is, the reversible reaction of esterification reaction) when it encounters water. Therefore, during storage, glyceryl triacetate will react with water in the product to form glyceryl monoacetate, glyceryl diacetate, Glycerin, acetic acid, etc., the acidity will gradually increase, causing the "return acid" of the sample, and finally lead to unqualified product quality
However, if alcohols such as ethanol are used to dilute triacetin, the alcohol can undergo transesterification, replace glycerin, generate esters such as ethyl acetate, and change the true content of monoacetin, diacetin and triacetin, thus affecting the quantitative accuracy

Method used

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  • A method for determining the content of glyceryl monoacetate and glyceryl diacetate in triacetin for cigarettes
  • A method for determining the content of glyceryl monoacetate and glyceryl diacetate in triacetin for cigarettes
  • A method for determining the content of glyceryl monoacetate and glyceryl diacetate in triacetin for cigarettes

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] Weigh 0.1000g of naphthalene (purity ≥ 99%) and dissolve it in a 1000ml volumetric flask, dilute to volume with anhydrous DMF, and use it as an internal standard solution for future use (internal standard concentration is 100 μg / ml).

[0031] Weigh 0.2500 g of glycerol triacetate (purity ≥ 99%) in a 250 ml volumetric flask, dilute to volume with anhydrous DMF, and use it as a standard stock solution for subsequent use (the concentration of the standard stock solution is 1.0 mg / ml). Pipette 1ml, 2ml, 3ml, 4ml, 5ml of standard stock solutions into 100ml Erlenmeyer flasks, add 20ml of internal standard solution, and mix well to obtain a series of standard working solutions.

[0032] The standard working solution was analyzed by gas chromatography mass spectrometer. The gas chromatographic conditions are: DB-5 fused silica capillary column (30m×0.53mm×1.5μm); inlet temperature: 260°C; temperature program: keep at 50°C for 1min, rise to 200°C at a rate of 5°C / min, Hold for ...

Embodiment 2

[0038] As described in Example 1, select another triacetin sample B, Figure 6 It is the chromatogram of triacetin sample B for cigarettes, and the sample is measured twice, and the content of monoacetin in triacetin sample B is 371.6mg / Kg, and the content of diacetin is 242.3mg / Kg.

[0039] Figure 5 , Figure 6 The retention time of 29.48min is the chromatographic peak of diacetin, and the retention time of 30.03min is the chromatographic peak of monoacetin.

[0040] The present invention uses anhydrous DMF as a solvent to dilute triacetin, avoiding the easy transesterification when diluting with alcohol solvents such as ethanol, and changing the true content of monoacetin, diacetin and triacetin, The phenomenon that affects the quantitative accuracy makes the analysis and detection results more accurate; adopts the high column capacity capillary chromatographic column with large pore diameter and thick liquid film to analyze triacetin samples, and realizes the simultaneou...

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Abstract

The invention provides a determination method for the content of glycerol monoacetate and glycerol diacetate in glycerol triacetate for cigarettes. The determination method comprises the following steps: (1) preparing an internal standard solution; (2) preparing a standard working solution; (3) determining by gas chromatography-mass spectrometry; (4) calculating a determination result of a sample.Aiming at the glycerol triacetate, the invention provides the determination method for analyzing the content of the glycerol monoacetate and the glycerol diacetate in the glycerol triacetate througha chromatographic column with a large pore diameter, a thick liquid film and a high column capacity by taking analytically pure anhydrous N,N-dimethylformamide as a solvent and directly diluting and feeding; the determination method has the advantages of convenience for operation, rapidness and the like.

Description

technical field [0001] The invention relates to the technical field of tobacco detection, in particular to a method for determining the content of glyceryl monoacetate and glyceryl diacetate in triacetin for tobacco. Background technique [0002] In the tobacco industry, glycerol triacetate is the main plasticizer used in the production of cigarette filter rods. On the one hand, it can solidify and form cellulose diacetate tow, thereby increasing filter rod hardness, pressure drop, thermal collapse resistance, and head shrinkage. and plasticity, etc., to obtain a filter stick that meets the needs of the cigarette tipping process; on the other hand, adding triacetin to the tow will affect the filtration efficiency of the filter stick and the smoking quality of the cigarette during the cigarette smoking process, reducing the The pungent, miscellaneous, choking, and spicy sensations in the smoke make the smoke plump and clean, and the taste is comfortable. [0003] Glycerol tr...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/88G01N30/06G01N30/60
CPCG01N30/06G01N30/60G01N30/88G01N2030/045G01N2030/884
Inventor 黄龙吴昭刘吟陈义坤刘磊
Owner HUBEI CHINA TOBACCO IND
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