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Solid-phase micro-extraction analysis method

A technology of solid-phase microextraction head and analysis method, applied in the field of solid-phase microextraction analysis, can solve the problems of reduced extraction efficiency, high incubation extraction temperature, unstable analyte, etc., and achieves simple and easy operation and easy online monitoring. Effect

Pending Publication Date: 2020-11-20
CHINA TOBACCO HUNAN INDAL CORP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the higher extraction temperature may also lead to the instability of the analyte, and the desorption temperature of the solid phase microextraction head is generally between 120 ° C and 280 ° C
The increase of extraction temperature will decrease the adsorption rate of the SPME head and increase the desorption rate. Therefore, increasing the extraction temperature may cause the adsorption and desorption of the SPME to be carried out at the same time, and will not increase the extraction efficiency.
Therefore, the recommended solid-phase microextraction temperature is generally below 100°C, but for the analysis of the aroma components of flavor samples, a higher incubation extraction temperature is often required. The equilibrium vapor pressure in the headspace sampling bottle increases further, especially when the temperature in the headspace sampling bottle rises above 120 °C, the soft cushion on the headspace sampling bottle cap It may burst, even if it does not burst, volatile gas is easy to overflow during the process of solid phase microextraction, resulting in a decrease in extraction efficiency

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0040] Take 0.2g of shredded tobacco into two 20ml headspace injection bottles respectively, and pump one of the headspace injection bottles with a 25ml syringe with an injection needle for several times until the pumping piston stops when it is difficult to pull. Coat the headspace bottle cushion with vacuum grease to serve as the experimental group; the control sample was not subjected to the above treatment, and the headspace sample bottle was placed in a heating furnace and heated to 250 ° C for 3 minutes. The experimental group bottle cap was intact, and the headspace of the control sample was intact. The soft cap of the vial cap burst and popped out.

Embodiment 2

[0042]Take 0.2g of shredded tobacco into two 20ml headspace sampling bottles respectively, connect one of the headspace sampling bottles to a circulating vacuum pump with a syringe with an injection needle and pump for a few minutes. After the pressure gauge of the vacuum pump is stable at 0.1mp, Put the sample into a heating furnace and heat it to 250 °C, keep it for 3 minutes, take out the headspace sampling bottle, and take it as the experimental group; Headspace solid-phase microextraction time was 50 min. Take out the solid-phase microextraction needle, and then perform analytical injection at the injection port of the gas chromatography-mass spectrometer. Compared with the control group, the information on the volatile components of the cut tobacco treated with negative pressure and high temperature is obviously rich, especially the types and contents of high-boiling components are significantly increased (see figure 1 , in general, the higher the boiling point, the lat...

Embodiment 3

[0044] Take 0.5g of dry soybean powder into two 20ml headspace injection vials, connect one of the headspace injection vials to a circulating vacuum pump with a syringe with an injection needle and pump for a few minutes. The pressure gauge of the vacuum pump is stable at 0.1mp. After that, put the sample into a heating furnace and heat it to 250 °C, keep it for 3 minutes, take out the headspace sampling bottle, and take it as the experimental group; 5min, headspace solid-phase microextraction time 30min. Take out the solid-phase microextraction needle, and then perform analytical injection at the injection port of the gas chromatography-mass spectrometer. Compared with the control group, the relative abundances of volatile components of soybean flour treated with negative pressure and high temperature were significantly enhanced, and the component information was significantly enriched.

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Abstract

The invention relates to a solid-phase micro-extraction analysis method which comprises the following steps of: putting a closed container filled with a to-be-analyzed substance and internally in a negative pressure state into an environment of 120-300 DEG C, heating for 1-15 minutes, taking out the closed container, and cooling the closed container to 60-120 DEG C; extracting the gas-phase components in the closed container by adopting a solid-phase micro-extraction technology to obtain an analysis sample; and carrying out chromatographic analysis on the obtained analysis sample, and collecting data. A sample is subjected to high-temperature heat treatment in a negative pressure state, aroma components in a distillation cracking area in the sample are extracted and then locked in a vacuumheadspace sample injection bottle, conventional solid-phase micro-extraction is then carried out, so that the temperature limitation of the solid-phase micro-extraction can be broken through, the high-boiling-point sample is realized at a relatively low solid-phase micro-extraction temperature, the operation is simple and feasible, the online monitoring is easy to realize, and a new way can be opened up for the solid-phase micro-extraction.

Description

technical field [0001] The invention relates to a solid-phase micro-extraction analysis method, in particular to a headspace solid-phase micro-extraction analysis method comprising negative pressure high temperature heat treatment, and relates to an analysis method of volatile components and / or semi-volatile components in samples. Background technique [0002] Solid-phase microextraction is a new type of sample processing method. It heats the sample into a headspace vial of a certain volume to volatilize volatile components from the sample, and then inserts the solid-phase microextraction head. Sampling, extraction, concentration and injection are integrated, and the operation is convenient; it has the advantages of high efficiency, simplicity and non-destructiveness. [0003] The main factors that affect solid-phase microextraction are: extraction temperature, extraction time, inorganic salts, pH and so on. For the volatilization efficiency of the sample, the higher the ex...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/06G01N30/12
CPCG01N30/02G01N30/06G01N30/12G01N2030/062G01N2030/126
Inventor 魏维伟黎艳玲杨华武黄平王威刘金云李亚白苏利霞朱卓越谭新良刘建福
Owner CHINA TOBACCO HUNAN INDAL CORP
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