Microextraction probe electrospray ion source and manufacturing method and application of microextraction probe electrospray ion source

An extraction and probe technology, applied in the chemical field, can solve the problems of unstable signal, short duration, and inability of spray solvent to infiltrate fibers effectively, and achieve the effect of strong selectivity and enrichment ability

Inactive Publication Date: 2014-11-05
SUN YAT SEN UNIV +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, because the surface of commercialized SPME fibers is usually hydrophobic, the spray solvent cannot effectively infiltrate the fibers, which easily leads to the disadvantages of unstable signal and short duration.

Method used

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  • Microextraction probe electrospray ion source and manufacturing method and application of microextraction probe electrospray ion source
  • Microextraction probe electrospray ion source and manufacturing method and application of microextraction probe electrospray ion source
  • Microextraction probe electrospray ion source and manufacturing method and application of microextraction probe electrospray ion source

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0052] The preparation of embodiment 1 microextraction probe

[0053] First cut the wood fiber into a length of about 2 cm, and then use a knife to further cut the tip of the wood fiber into a thinner tip (0.1-0.2 mm in outer diameter, which is similar to the capillary size of a commercial electrospray ion source). Wood fiber matrices for microextraction probes. Then, the wood fiber matrix was placed in a two-necked flask, and 100 mL of anhydrous N,N-dimethylformamide and 5 mL of dimethyloctadecyl[3-(trimethoxysilyl)propyl]chloride were added Ammonium, nitrogen, heated to 120 ° C, stirred and refluxed for 12 hours. After the reaction was completed, the wood fiber matrix with the adsorption material bonded on the surface was repeatedly washed with methanol three times, and dried naturally to obtain the micro-extraction probe.

Embodiment 2

[0054] The characterization of the microextraction probe of embodiment 2

[0055] Figure 5 The photoelectron spectroscopy of the microextraction probe surface is shown, from which C-, O-, N- and Si-related peaks can be observed. The content percentage of Si and N in the surface-bonded wood fiber matrix is ​​2.14%-2.35%. The Si2p peak shows Si-CH at a binding energy of 102.8eV 2 bond and the Si-O bond at 102.2eV ( Figure 5-2 ), the N1s peak shows the N-CH with binding energy at 399.6eV 2 key and N-CH of 402.2 3 key( Figure 5-3 ). Through photoelectron spectroscopy analysis, it was confirmed that the silyl group of dimethyloctadecyl [3-(trimethoxysilyl) propyl] ammonium chloride was bonded to the hydroxyl group on the surface of the wood fiber matrix through a silanization reaction.

[0056] Figure 6 Shown are the scanning electron micrographs of the unmodified wood fiber matrix and the microextraction probe of the present invention. It can be clearly shown in the fi...

Embodiment 3

[0057] Example 3 Extraction and Microextraction Probe Electrospray Mass Spectrometry Analysis

[0058] The operation mode of sample extraction is consistent with that of solid-phase microextraction, and the mode of direct extraction is adopted. Before extraction, the microextraction probe was rinsed with methanol for 30 s. After the extraction, the micro-extraction probe was quickly taken out from the sample, then rinsed in pure water for 10 seconds and then taken out, and then the micro-extraction probe was analyzed by electrospray mass spectrometry after natural drying.

[0059] The extracted micro-extraction probe was fixed on the three-dimensional mobile stage, so that the tip of the micro-extraction probe was aligned with the entrance of the mass spectrometer and was 10 mm away from the entrance of the mass spectrometer. An external –3.5kV high-voltage electric field is loaded on the micro-extraction probe, and then 5 μL of methanol spray solvent is added dropwise on the...

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Abstract

The invention belongs to the field of chemistry, and relates to a microextraction probe electrospray ion source and a manufacturing method and application of the microextraction probe electrospray ion source, in particular to a probe capable of being directly used for complex-matrix solid-phase microextraction and direct-electrospray mass spectrometry analysis and a manufacturing method and application of the probe. The probe is characterized in that a silanization reaction is carried out on adsorption materials containing silylation and pointed-shaped wood fiber matrixes with the surface rich in hydroxyl, and the microextraction probe is obtained. By means of the probe, high enrichment coefficients of trace target compounds in multiple kinds of complex matrixes can be directly extracted, the probe after extraction can carry out direct electrospray to ionize the target compounds in the normal-pressure open environment and carry out mass spectrometry analysis; the microextraction electrospray probe achieves solid-phase microextraction and ambient mass spectrometry combination analysis, can be used as the novel electrospray ion source and has the high sensitivity and the ideal reproducibility.

Description

technical field [0001] The invention belongs to the field of chemistry, and relates to a micro-extraction electrospray probe and its preparation and application, in particular to a probe which can be directly used for complex matrix solid-phase microextraction and direct electrospray mass spectrometry analysis, and its preparation method and application . Background technique [0002] Solid-phase microextraction (SPME) is a pretreatment technology integrating sampling, extraction, concentration and sample injection. It uses physical or chemical methods to immobilize the coating material with adsorption and extraction functions on the surface of a certain matrix, and the sample Through direct or indirect contact, the target analyte is enriched and concentrated, and then desorbed to analyze the target analyte in the sample. It has the advantages of small sample consumption and high selectivity. The properties of the SPME coating material determine the extraction capacity, se...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): H01J49/16G01N27/62C07F7/18
CPCH01J49/165H01J49/0431
Inventor 杨运云邓洁薇栾天罡方玲
Owner SUN YAT SEN UNIV
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