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Combined thermal desorption solid-phase extraction bar preparation and application method for GC/MS

An extraction rod and thermal desorption technology, applied in the field of chromatographic separation, can solve problems such as inability to fully inject samples, solvent peak interference, and low sensitivity, and achieve the effects of shortening pretreatment time, easy assembly, and improving detection sensitivity

Inactive Publication Date: 2019-08-13
APPLE FLAVOR & FRAGRANCE GRP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] Most of the existing extraction technologies use the method of "extraction adsorption-elution with eluent" to collect the required substances for detection, but this method has the disadvantages of not being able to inject all samples, low sensitivity, and complicated operation. In addition, during the separation process of gas chromatography, Trace components with short retention times are easily interfered or even overwhelmed by solvent peaks

Method used

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  • Combined thermal desorption solid-phase extraction bar preparation and application method for GC/MS
  • Combined thermal desorption solid-phase extraction bar preparation and application method for GC/MS
  • Combined thermal desorption solid-phase extraction bar preparation and application method for GC/MS

Examples

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Effect test

Embodiment 1

[0034] GC / MS Analysis of a Perfume Sample

[0035] 1. Preparation of solid phase extraction stick:

[0036] (1) The solid phase extraction rod is made of glass, and its shape is a rod with two hemispheres (see figure 1 ,), whose size is 2mm in diameter and 3cm in length

[0037] (2) Cleaning and pretreatment of extraction rods:

[0038] use CH 2 Cl 2 Clean the glass extraction rod, and then treat it with 1mol / L NaOH solution for 8 hours to expose the silanol on the glass surface, treat it with 0.1mol / L hydrochloric acid solution for 8 hours, and then wash it with deionized water until neutral. Under the protection of nitrogen, dry the glass extraction rod at 100°C-190°C for later use.

[0039] (3) Surface coating:

[0040] The polydimethylsiloxane solution was coated on the glass surface by sol-gel method, aged and fixed in an aging device (300°C, heated for 4h). The adsorption rod was activated with 6 mL of acetone at a flow rate of 2 drops·S -1 .

[0041] (4) Surfac...

Embodiment 2

[0048] GC / MS analysis of water-extracted samples of Tongkat Ali

[0049] The difference from Example 1 is that the material of the solid-phase extraction rod is metal, such as: copper or stainless steel or aluminum. The material of the solid-phase extraction rod in this embodiment is copper. The specific steps are as follows:

[0050] 1. Preparation of solid-phase extraction sticks

[0051] (1) The solid phase extraction rod is made of copper, and its shape is an ellipsoid rod (see figure 2 ) with a maximum diameter of 2 mm and a length of 3 cm.

[0052] (2) Pretreatment of the extraction rod: the surface of the metal rod is etched by the electrochemical anodic dissolution method, the ellipsoidal copper rod is used as the anode, the graphite electrode is used as the cathode, phosphoric acid / sodium phosphate (pH 5) is used as the electrolyte, and 5V DC , electrolysis 5min. Take out the metal rod, rinse it with deionized water until neutral, and dry the metal rod at 100°C to...

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Abstract

The invention relates to a combined thermal desorption solid-phase extraction bar preparation and application method for gas chromatography / mass spectrum (GC / MS). Extraction bars of different structures, in different sizes and with different adsorption functions are prepared, and the extraction bars can be used for adsorbing samples of different structures or in various types. The extraction barsare placed in a thermal desorption tube at the same time, and after one-time thermal desorption, the adsorbed samples are all desorbed; all the samples are directly conveyed into the GC / MS for analysis to obtain more sample information. The method has the advantages that according to different detection requirements, during adsorption and desorption, one thermal desorption solid-phase extraction bar is used or various adsorption bars are used at the same time. Besides, in order to improve the detection effect of one certain kind of substance, multiple adsorption bars can be used at the same time for adsorption to improve the adsorption capacity, and the detection sensitivity for specific substances is improved. The thermal desorption solid-phase extraction bars have the advantages of beingsimple in structure and easy to assemble.

Description

technical field [0001] The invention relates to the technical field of chromatographic separation, in particular to a method for preparing and using a combined thermal desorption solid-phase extraction rod for gas chromatography / mass spectrometry (GC / MS). Background technique [0002] Solid phase extraction is a two-phase physical extraction process including liquid phase and solid phase. It is a separation and extraction technology developed on the basis of liquid-solid extraction and liquid chromatography. This technology mainly uses the difference in adsorption between different compounds and adsorbents when the sample flows through the solid adsorbent to separate the specific analyte in the liquid sample from the sample substrate and interfering compounds, and then quickly elute through the eluent. To achieve the effect of separation and enrichment. The use of solid-phase extraction for sample treatment can not only effectively remove impurities, but also increase the c...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J20/281B01J20/30B01D15/10G01N30/06
CPCB01D15/10B01J20/281B01J2220/52B01J2220/86G01N30/06G01N2030/062
Inventor 庄伟强康维君张凌怡张维冰
Owner APPLE FLAVOR & FRAGRANCE GRP
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