Method for measuring formaldehyde, acetaldehyde and acetone in tobacco water-based adhesive by derivatization-headspace gas chromatography
A technology of headspace gas chromatography and tobacco water-based glue, which is applied in the direction of measuring devices, instruments, scientific instruments, etc., can solve the problems of high-performance liquid chromatography analysis applications, organic solvents are not environmentally friendly, and phenylhydrazone is easy to hydrolyze, etc., to achieve simplification Pre-treatment process, no consumption of organic solvent, effect of reducing pollution
Active Publication Date: 2017-09-01
CHINA TOBACCO ZHEJIANG IND
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Among them, the sample is derivatized by 2,4-dinitrophenylhydrazine to phenylhydrazone, and HPLC analysis is the most widely used. In the acidic environment required for the derivatization reaction, phenylhydrazone is easily hydrolyzed, resulting in a decrease in the measured value.
Gas chromatography analysis needs to be pre-treated with derivative reagents such as pentafluorobenzyl hydroxylamine (PFBHA) and pentafluorophenylhydrazine, and then the derivative product is transferred to the organic phase through an organic solvent for GC analysis. The operation is cumbersome and consumes too much organic solvent. Disadvantages such as environmental protection
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Embodiment 1
[0040] 1 Experimental part
[0041] 1.1 Materials, reagents and instruments
[0042] Water-based adhesive samples (provided by Zhejiang China Tobacco Industrial Co., Ltd.). Formaldehyde, acetaldehyde, acetone single standard solution (1.0mg / mL, Bailingwei Technology Co., Ltd.); pentafluorobenzyl hydroxylamine standard (Tokyo Chemical Industry Co., Ltd.). Model 7890 gas chromatograph (with HP-7697A headspace sampler), HP-5 chromatographic column (30m×0.25mm×0.25μm) (Agilent, USA); AG104 electronic balance (sensitivity 0.0001g, Swiss Metter-Toledo company); Milli-Q Advantage A10 ultrapure water system (Millipore, USA); vortex mixer (Qilin Bell Instrument Co., Ltd. Haimen); Sigma 4-16k high-speed centrifuge (Sigma, Germany).
[0043] 1.2 Prepare mixed standard stock solution, mixed standard working solution and derivative reagent solution. : Accurately weigh 1.0mL formaldehyde standard solution, 5.0mL acetaldehyde standard solution, and 5.0mL acetone standard solution, and use...
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Abstract
The invention discloses a method for measuring formaldehyde, acetaldehyde and acetone in tobacco water-based adhesive by derivative-headspace gas chromatography, which comprises the following steps: (1) dispersing tobacco water-based adhesive in deionized water proportionally, shaking for extraction, centrifuging, collecting supernatant, adding into a headspace bottle, adding a derivatization reagent (water solution of pentafluorobenzyl hydroxylamine) proportionally, performing gland sealing, mixing, and performing headspace gas chromatography; and (2) drawing a standard curve of chromatogram peak area of a target analyte vs. concentration thereof, introducing the chromatographic results obtained in step (1) into the corresponding standard curve, and calculating the concentrations of formaldehyde, acetaldehyde and acetone in tobacco water-based adhesive. The invention establishes a simple and rapid method for accurately measuring formaldehyde, acetaldehyde and acetone in tobacco water-based adhesive by derivative-headspace gas chromatography. The method of the invention is simple, rapid and accurate, realizes automation, and does not consume organic solvent.
Description
technical field [0001] The invention belongs to the technical field of detection of harmful substances in tobacco water-based glue, and particularly relates to a method for determining formaldehyde, acetaldehyde and acetone in tobacco water-based glue by derivatization-headspace gas chromatography, specifically using water as a matrix Calibration agent, derived from pentafluorobenzyl hydroxylamine, under a certain equilibrium temperature and equilibrium time, the method is determined by headspace-gas chromatography (HS-GC). Background technique [0002] Carbonyl compounds such as aldehydes and ketones, as harmful substances, have long received attention in environmental and biochemical research. Long-term exposure to high levels of aldehydes and ketones can easily lead to lung diseases, Alzheimer's, cancer and other diseases. As an important smoking material, water-based adhesives have been highly valued by the tobacco industry in recent years for their safety and hygiene, ...
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IPC IPC(8): G01N30/06
CPCG01N30/06G01N2030/067
Inventor 游金清陆成飞乔跃辉林建南刘博倪建彬李茂松柴武君
Owner CHINA TOBACCO ZHEJIANG IND
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