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Reagent for deriving small molecule aldehyde material and use thereof

A derivatization reagent and molecular aldehyde technology, applied in the field of analytical chemistry, can solve the problems of poor selectivity of target analytes, obvious interference of impurity components, increase the difficulty of analysis, etc., and achieve the effects of fast derivatization, simple preparation and low price

Active Publication Date: 2011-11-09
ZHENGZHOU TOBACCO RES INST OF CNTC
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The sample capture process of this analysis method is complicated, the selectivity to the target analyte is poor, the interference of impurity components is obvious, and the derivatization with 2,4-dinitrophenylhydrazine requires a long derivatization time
Studies have found that derivatization of small molecule aldehydes with 2,4-dinitrophenylhydrazine will introduce impurities, which will interfere with the analysis and increase the difficulty of analysis

Method used

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  • Reagent for deriving small molecule aldehyde material and use thereof
  • Reagent for deriving small molecule aldehyde material and use thereof
  • Reagent for deriving small molecule aldehyde material and use thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0012] Selective analysis of small molecule aldehydes in the air: 7% diphenylamine, 35% DHB and 58% ethylene glycol were formulated as reagent (A) for derivatization of small molecule aldehydes according to the method provided by the present invention. Use a micro-syringe to absorb 2 μL of the derivatization reagent A, insert the needle of the micro-syringe into the headspace bottle that collects the air sample to be tested; carefully depress the plunger of the micro-syringe to expose the derivatization reagent to the headspace bottle, extract and derivatize After 1.5 min; suck back the droplet, drop the droplet onto the MALDI target of matrix-assisted laser desorption ionization (MALDI) Fourier transform mass spectrometry, and perform mass spectrometry analysis directly after the droplet dries to determine the aldehyde compounds (Table 1).

[0013] Table 1 adopts the derivatization reagent of the present invention to analyze the result of aldehydes in flue gas

[0014]

Embodiment 2

[0016] Quantitative analysis of formaldehyde and acrolein in flue gas: 5% diphenylamine, 35% DHB and 60% ethanol were formulated as reagent (B) for derivatization of small molecule aldehydes according to the method provided by the present invention. Take a certain amount of internal standard (tetrabutylammonium bromide) solution and mix with derivatization reagent to form solution C. Use a micro-syringe to absorb 1 μL of the derivatization reagent C, insert the needle of the micro-syringe into the headspace bottle where the smoke sample to be tested is collected; carefully press down the plunger of the micro-syringe to expose the derivatization reagent to the headspace bottle, extract and The derivatization time is 1min; the droplet is sucked back, and the droplet is added to the MALDI target of matrix-assisted laser desorption ionization (MALDI) Fourier transform mass spectrometry. The relative abundance of the substance was regressed to the amount of aldehyde to obtain the c...

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Abstract

The invention relates to reagent for the derivatization of small molecular aldehyde substance and application thereof. The invention is characterized in that the reagent is composed of the substances in the following weight ratio: 1 - 10 percent of diphenylamine, 20 - 40 percent of 2,5-dihydroxy benzoic acid and 50 - 60 percent of alcohol. The derivative process reagent is utilized as extraction solution for liquid-phase micro-extraction (LPME), the small molecular aldehyde in the gas phase of the flue gas is directly extracted and derived through the LPME method, after the extraction is finished, the derivatization of the small molecular aldehyde substance is simultaneously finished, the solution with extracted analyte is directly dropped to the target plate of MALDI mass spectrum, the analysis is directly performed after the solution is air dried, therefore, qualitative detection or quantitative detection can be performed for the aldehyde compound, and extra matrix for the MALDI mass spectrum is not required. The invention has the advantages that the selectivity is strong and the sensitivity is high, the diction limit for formaldehyde and acrolein can reach fmol level; the preparation is simple, and the cost is low.

Description

technical field [0001] The invention belongs to the field of analytical chemistry, and in particular relates to a reagent for derivatization of small-molecule aldehydes and an application thereof, which can analyze and measure small-molecule aldehydes in cigarette smoke. Background technique [0002] Small molecule aldehydes (mainly formaldehyde, acetaldehyde and acrolein, etc.) have cilia toxicity and are a class of harmful substances in the environment. Smoke produced by burning cigarettes is an important source of small molecule aldehydes in indoor air, so the analysis and research of small molecule aldehydes in cigarette smoke has always been concerned by analysts. Due to the small molecular weight, strong volatility, and high polarity of small molecule aldehydes, it is difficult to collect them and cannot be directly analyzed by instruments. Usually, derivatization techniques are used before chromatographic analysis. At present, the commonly used analysis method is mai...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/06G01N27/64
Inventor 谢剑平孙世豪尹杰宗永立
Owner ZHENGZHOU TOBACCO RES INST OF CNTC
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