Solid-phase extraction-gas chromatography and mass spectrometry combined separation and detection method for discharge of organic acid by biomass combustion in snow ice sample

A technology of gas chromatography mass spectrometry and detection method, which is applied in the field of solid phase extraction-gas chromatography mass spectrometry combined separation and detection, can solve the problems of low detection limit, large sample volume and high detection limit, and achieves reduction of ionization degree and improvement of recovery. rate, the effect of promoting protonation

Inactive Publication Date: 2017-05-24
中国科学院青藏高原研究所
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Problems solved by technology

This method has a low detection limit, but the operation is relatively complicated, it cannot be operated in the field, a large amount of sample is required, and a large amount of organic reagents are consumed in the extraction process
The other is to use HPLC-ESI-MS/MS to measure organic acids directly. This method has the ch...

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  • Solid-phase extraction-gas chromatography and mass spectrometry combined separation and detection method for discharge of organic acid by biomass combustion in snow ice sample
  • Solid-phase extraction-gas chromatography and mass spectrometry combined separation and detection method for discharge of organic acid by biomass combustion in snow ice sample

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Effect test

Embodiment 1

[0045] Assay compound:

[0046] Three organic acids emitted from biomass combustion in snow and ice: p-hydroxybenzoic acid, vanillic acid, and dehydroabietic acid.

[0047] Method validity:

[0048] The concentration corresponding to three times the standard deviation of the Milli-Q ultrapure water full-process blank six repeated measurements was used as the minimum detection limit of the method, which were: p-hydroxybenzoic acid 0.002ng / mL, vanillic acid 0.001ng / mL mL, dehydroabietic acid 0.004ng / mL, and if a larger sample volume is used, a lower detection limit can be obtained. 1.0ng / mL standard solution is used to test the recovery of the method, and the results show that the recovery of the three organic acids is all greater than 75%, and the relative standard deviation (RSD) of the measured value (n=6) is all less than 15% (see table 1).

[0049] Actual sample determination process:

[0050] The concentration levels of p-hydroxybenzoic acid, vanillic acid and dehydroa...

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Abstract

A solid-phase extraction-gas chromatography and mass spectrometry combined separation and detection method for discharge of organic acid by biomass combustion in a snow ice sample comprises the following steps: preparing a sample: filtering the sample with a quartz filter membrane; performing SPE preparation: fixing an HLB small column on a special SPE device; activating the HLB small column; adjusting the PH value: taking 50 mL of filtered sample, adding hydrochloric acid (PH is about 2) and shaking uniformly; loading the sample: adding the sample which is shaken uniformly into the HLB column; leaching and blow-drying; eluting and collecting eluent; concentrating; determining the volume and putting on a machine: after deriving and cooling to room temperature, adding normal hexane, determining the volume to be 200 mL and preparing to put on a gas chromatograph-mass spectrometer (GC/MS) to perform test. The detection method provided by the invention has the characteristics of small use amount of the samples, high field operability, simplicity in operation and the like; furthermore, the detection method has low detection limit, high recovery rate and high precision.

Description

technical field [0001] The invention relates to a method for detecting chemical components of snow and ice, in particular to a solid phase extraction-gas chromatography mass spectrometry separation and detection method for organic acids emitted from biomass combustion in snow and ice samples. Background technique [0002] p-Hydroxybenzoic acid, vanillic acid, and dehydroabietic acid in snow and ice are unique indicators of biomass combustion emissions, which can be used to distinguish whether carbonaceous components come from biomass combustion or fossil fuel combustion. However, snow and ice samples There are still very few studies on medium organic acids as indicators of combustion emissions, the main reason being the limitations of sample pretreatment methods and instruments. [0003] At present, there are mainly two methods for the separation and analysis of organic acids in snow and ice that can be used as combustion emission indicators: one is to collect a large number...

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Application Information

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IPC IPC(8): G01N30/88
Inventor 高少鹏丛志远康世昌武广明
Owner 中国科学院青藏高原研究所
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