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Detection method and device for volatile and semi-volatile components

A semi-volatile, detection method technology, applied in the field of chemistry, can solve the problems of unsuitable chromatography mode, unsuitable for volatile components, etc., and achieve the effect of improving analytical sensitivity

Inactive Publication Date: 2013-09-04
YUNNAN RES INST OF TOBACCO SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] At present, the solvent treatment of traditional liquid-gas two-dimensional chromatography adopts vacuum solvent evaporation technology, which is not suitable for volatile components, and is not suitable for primary chromatography.

Method used

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  • Detection method and device for volatile and semi-volatile components
  • Detection method and device for volatile and semi-volatile components
  • Detection method and device for volatile and semi-volatile components

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0040] Take 20 domestic flue-cured cigarette samples to collect the total particle phase of the smoke according to the method of GB / T 19609-2004, put the obtained filter into the conical flask, and accurately add 1ml of the third-level internal standard with a pipette Solution, accurately add 40ml cyclohexane. Place in an ultrasonic generator for ultrasonic extraction for 40 minutes (ultrasonic frequency 60%), cool to room temperature, take 10 mL of the extract and concentrate it to 1.0 mL, put it into a chromatographic bottle for liquid chromatography separation. Start the liquid chromatograph, the injection volume is 20 μL, the sample enters the liquid chromatographic system, the mobile phase is delivered by pump A and separated by the liquid chromatographic column separation column, and the effluent components of 6 - 6.5 min pass through the digital control six-way The valve cuts into the catch coil and the remainder drains into the waste bottle. Start the pump B, and the ...

Embodiment 2

[0042] Take 20 samples of foreign blended cigarettes and collect the total particulate matter in the smoke according to the method of GB / T 19609-2004, put the obtained filter into the conical flask, and accurately add 1ml of the third-level internal standard with a pipette Solution, accurately add 40ml cyclohexane. Place in an ultrasonic generator for ultrasonic extraction for 40 minutes (ultrasonic frequency 60%), cool to room temperature, take 10 mL of the extract and concentrate it to 1.0 mL, put it into a chromatographic bottle for liquid chromatography separation. Start the liquid chromatograph, the injection volume is 20 μL, the sample enters the liquid chromatographic system, the mobile phase is delivered by pump A and separated by the liquid chromatographic column separation column, and the effluent components of 6 - 6.5 min pass through the digital control six-way The valve cuts into the catch coil and the remainder drains into the waste bottle. Start the pump B, and...

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Abstract

The invention discloses a detection method and a device for volatile and semi-volatile components. The detection method for the volatile and semi-volatile components comprises the steps of collecting, preparing and analyzing samples and especially comprises the following steps of: performing catching by a filter disc, adding an organic solvent, and performing ultrasonic oscillation to obtain the sample; and performing liquid chromatographic separation on the sample, cutting flow-out components into a catching coil pipe, conveying the sample in the catching coil pipe into a gas chromatography (GC) device, adsorbing the sample by a solid phase extraction column, starting a gas chromatography-mass spectrometer (GC-MS), and analyzing components to be measured in a capillary separation column. The device is a liquid and gas phase bi-dimensional chromatography device, and solvent treatment between the liquid chromatography (LC) device and the gas chromatography device is solid phase extraction. According to the method and the device, the sample can enter a first-level LC with a large size, and fractions of the first-level LC can be cut into a second-level GC with a large size, so that as for the low-content samples, components separated by LC can be accumulated for many times, and then are transferred into the GC for analysis after being accumulated to an ideal analysis amount. Therefore, the samples can be efficiently purified, and the analysis sensitivity is greatly improved.

Description

technical field [0001] The invention belongs to the technical field of chemistry, and in particular relates to a detection method and a device for volatile and semi-volatile components. Background technique [0002] Liquid-gas two-dimensional chromatography is a new technology developed in recent years. Because liquid chromatography can provide good group separation, it can perform purification and enrichment on samples, while gas chromatography has high separation ability. and high analysis speed, the samples can be further separated and analyzed. The combination of the two enables the advantages of the two chromatography to be fully utilized; on the other hand, through automatic online coupling, the manual pretreatment of samples is greatly reduced. Human error is avoided. This not only improves the reliability of the analytical method, but also saves time, and complex analysis can be made simple and convenient in this way. However, due to the microliter injection volume...

Claims

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Application Information

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IPC IPC(8): G01N30/46
Inventor 孔维松张霞杨光宇韩熠段沅杏陈永宽缪明明
Owner YUNNAN RES INST OF TOBACCO SCI
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