Method for determining 1,1,1-trimethylolpropane in tobacco paper

A technology for the determination of trimethylolpropane and its method, which is applied in the field of determination of 1,1,1-trimethylolpropane in cigarette paper

Active Publication Date: 2014-10-29
CHINA NAT TOBACCO QUALITY SUPERVISION & TEST CENT
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The pretreatment of the above methods requires complex and cumbersome steps such as degradation, esterification, and reflux. Since the TMP content is very low, the sensitivity is not high enough.

Method used

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  • Method for determining 1,1,1-trimethylolpropane in tobacco paper
  • Method for determining 1,1,1-trimethylolpropane in tobacco paper

Examples

Experimental program
Comparison scheme
Effect test

example 1

[0036] 1. Instruments and reagents:

[0037] 1,1,1-Trimethylolpropane and methanol are chromatographic grade reagents; ultrapure water meets the requirements of first-grade water in GB / T 6682.

[0038] API 4000 quadrupole tandem mass spectrometer; Swiss Mettler AE 163 electronic balance (sensitivity: 0.0001g).

[0039] 2. Sample handling:

[0040] Accurately weigh 1.0 g of the sample; place it in a 50 mL Erlenmeyer flask with a stopper, add 20 mL of ultrapure water accurately, ultrasonically extract for 30 min; let stand for 5 min, pipette 8 mL of the extract into a 10 mL centrifuge tube , centrifuged at 10000 rpm for 10 min. Aspirate the supernatant and filter it through a 0.22 μm organic phase filter. Pipette 100 μL of the filtrate, dilute the sample to 1.0 mL with ultrapure water, and conduct LC-MS / MS analysis.

[0041] 3. Prepare the standard working solution: Accurately weigh 10 mg of 1,1,1-trimethylolpropane into a 10 mL volumetric flask, accurate to 0.1 mg, dissol...

example 2

[0046] According to the method described in Example 1, another tipping paper sample for cigarettes was selected, and the content of 1,1,1-trimethylolpropane was not detected in the sample.

example 3

[0048] According to the method described in Example 1, another sample of inner liner paper for cigarettes was selected, and the content of 1,1,1-trimethylolpropane in the sample was measured to be 0.41 mg / kg.

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Abstract

The invention belongs to the technical field of physical and chemical inspection of hazardous substances remained in tobacco paper, and in particular relates to a method for determining 1,1,1-trimethylolpropane in tobacco paper. The method is characterized by comprising the steps: cutting the tobacco paper into pieces, adding ultrapure water for carrying out ultrasonic extraction, and directly determining the 1,1,1-trimethylolpropane in the tobacco paper by adopting a liquid chromatogram- tandem mass spectrum after an extraction solution is centrifuged. The method can rapidly and accurately detect the residual amount of the 1,1,1-trimethylolpropane in the paper and has the advantages of being accurate in determination result, low in determining interference, high in sensitivity and good in repeatability.

Description

[0001] technical field [0002] The invention belongs to the technical field of physical and chemical inspection of harmful substance residues in cigarette paper, and mainly relates to a method for measuring 1,1,1-trimethylolpropane in cigarette inner liner paper, tipping paper and carton wrapping paper, specifically It is a method of ultrasonically extracting 1,1,1-trimethylolpropane and directly determining it by liquid chromatography-tandem mass spectrometry. [0003] Background technique [0004] 1,1,1-Trihydroxymethylpropane (TMP) is a white flaky crystal, easily soluble in water, lower alcohols, glycerol, dimethylformamide, partially soluble in ethyl acetate, acetone, slightly soluble in Diethyl ether, chloroform, carbon tetrachloride, insoluble in aliphatic hydrocarbons, aromatic hydrocarbons and chlorinated hydrocarbons. There are three typical methylol groups on the molecule of trimethylolpropane, so it has the properties of polyols similar to glycerol, and is a w...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02
Inventor 杨飞李中皓边照阳范子彦刘珊珊张洪非王颖张艳革唐纲岭胡清源
Owner CHINA NAT TOBACCO QUALITY SUPERVISION & TEST CENT
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