Matrix Matching Calibration-Headspace Gas Chromatography Determination of Menthol Content in Acetate Filter Sticks
A headspace gas chromatography and matrix matching technology is applied in the field of cigarette detection, which can solve the problems of increasing the sample size and difficulty of menthol analysis, affecting the quality of filter rods and cigarettes, and a large amount of organic solvents, achieving high-throughput automatic analysis, The effect of easy automation and low solvent consumption
Active Publication Date: 2015-09-02
CHINA TOBACCO ZHEJIANG IND
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Problems solved by technology
During production and storage, even in small packs of cigarettes, the menthol in the filter stick is volatile and causes loss, which affects the quality of the filter stick and cigarettes, and also increases the sample size and analysis difficulty of menthol analysis
The tobacco industry standard "YC / T 416-2011 Determination of Menthol in Fiber Acetate Filter Stick by Gas Chromatography" and the invention patent "Determination of Menthol in Cigarette Filter Stick" (Patent No.: 201110197167) use mechanical vibration extraction, which is cumbersome to operate and require large amounts of organic solvents
There is no report on headspace gas chromatography for the determination of menthol in filter sticks
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[0014] The following examples are intended to further illustrate the present invention, rather than limit the present invention.
[0015] The method for matrix matching correction-Headgas Gas Chromatography Determination of Menthol Content in Acetate Filter Stick, the method may further comprise the steps:
[0016] 1) Preparation of internal standard solution, standard stock solution, and standard working solution: Accurately weigh 0.5 g of phenylethyl propionate into a 500 mL volumetric flask, dilute with DMF (N,N-dimethylformamide) to obtain the internal standard solution (1mg / mL internal standard). Weigh 1.0 g of menthol and 0.1 g of phenylethyl propionate into a 100 mL volumetric flask, dilute to volume with DMF to obtain a standard stock solution (10 mg / mL menthol). Pipette an appropriate amount of standard stock solution and dilute it with internal standard solution to form standard working solutions of 0.1, 0.25, 0.50, 1.0, 2.0, 5.0 mg / mL.
[0017] 2) Sample pretreatm...
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The invention relates to a method for testing content of menthol in an acetate fiber filter stick through matrix matching correction-headspace gas chromatography. The method comprises the following steps: 1) preparing an interior label liquid, a standard storage liquid and a standard working solution; 2) pretreating a sample, namely, peeling off cut tobacco and paper from a cigarette sample, putting a filter tip into a headspace bottle of 20 mL, adding the interior label liquid, sealing by using a gland and subsequently feeding the sample; 3) testing the sample by using an Agilent headspace gas chromatographic instrument; 4) determining the nature and quantifying, namely, determining the nature according to a standard sample retaining time, a single fed standard sample and a chromatogram of a blank solution, the standard solution and a practical sample solution, quantifying by using an internal label method, and drawing a standard working curve by using a peak area ratio y and a concentration ratio of the menthol to the internal label to obtain corresponding retaining time, a linear equation, detected limit and detection limit. The method adopts headspace sample feeding, the pretreatment on the sample is simple and easy to realize automation, and the method has the advantages of simplicity, rapidness, accuracy, automation, wide application range and the like.
Description
technical field [0001] The invention relates to the field of cigarette detection, in particular to a method for determining the menthol content in cellulose acetate filter rods by matrix matching correction-headspace gas chromatography. Background technique [0002] Menthol is without a doubt the most popular flavor of cigarettes. Adding menthol to the filter stick is an important means of producing menthol cigarettes. During production and storage, even in small packs of cigarettes, the menthol in the filter stick is volatile and causes loss, which affects the quality of the filter stick and cigarettes, and also increases the sample size and analysis difficulty in menthol analysis. The tobacco industry standard "YC / T 416-2011 Determination of Menthol in Fiber Acetate Filter Stick by Gas Chromatography" and the invention patent "Determination of Menthol in Cigarette Filter Stick" (Patent No.: 201110197167) use mechanical vibration extraction, which is cumbersome to operate ...
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IPC IPC(8): G01N30/88
Inventor 游金清倪建彬
Owner CHINA TOBACCO ZHEJIANG IND