Solid-phase extraction column used cooperatively with GC-FID instrument and application thereof

A GC-FID, solid phase extraction column technology, applied in the detection of mineral oil contaminants in food, detection of mineral oil contaminants in food systems field, can solve the LVI sampling system stability and repeatability is not ideal, solid phase The application of extraction column is limited, and the solid-phase extraction column needs to be improved to achieve the effect of easy promotion, improved repeatability and accuracy, and good versatility

Inactive Publication Date: 2016-03-30
BEIJING CENT FOR PHYSICAL & CHEM ANALYSIS
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] At present, there is no special sample pretreatment SPE column for the analysis of mineral oil in food on the market. Due to the problems of column material, capacity and column packing, the SPE column made by some laboratories has poor pollution and purification effect. The capacity is too small, and the subsequent GC-FID analysis of mineral oil must use a large volume injection device (LVI) to obtain better sensitivity and detection limit
However, currently there are very few detection units and departments with LVI-GC-FID, and the stability and repeatability of the LVI sampling system are not ideal
Therefore, the application of this solid phase extraction column is limited
[0006] Therefore, in the current research field of quantitative analysis of mineral oil pollutants in food, the solid phase extraction column for pretreatment of the samples to be tested for the detection of food mineral oil pollutants still needs to be improved.

Method used

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  • Solid-phase extraction column used cooperatively with GC-FID instrument and application thereof
  • Solid-phase extraction column used cooperatively with GC-FID instrument and application thereof
  • Solid-phase extraction column used cooperatively with GC-FID instrument and application thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0080] Prepare the solid phase extraction column 1000 (such as Figure 16 shown):

[0081] (1) Prepare a 50mL glass chromatography column (i.e. hollow glass column 100). The bottom of the column tube is provided with an extraction column outlet, and a glass fiber sieve plate 101 is sintered close to the bottom of the column, and a glass fiber upper sieve plate matching the glass column is processed at the same time. 101 (pore diameter 10μm, thickness 1mm).

[0082] (2) Activated alumina: bake alumina with a particle size of 60 μm in a muffle furnace at 500° C. for 4 hours, and put it in a desiccator for later use.

[0083] (3) Activated silica gel: bake silica gel with a particle size of 60 μm in a muffle furnace at 500° C. for 4 hours, take it out after cooling, and put it in a desiccator for later use.

[0084] (4) Preparation of silver nitrate-stained silica gel: Accurately weigh analytically pure silver nitrate in a volumetric flask, dissolve it with distilled water and ...

Embodiment 2

[0088] Prepare the solid phase extraction column 1000 (such as Figure 16 shown):

[0089] (1) Prepare a 100mL glass chromatography column (i.e., a hollow glass column 100). The bottom of the column tube is provided with an outlet of the extraction column, and a glass fiber sieve plate 101 is sintered close to the bottom of the column, and a glass fiber upper sieve plate matching the glass column is processed at the same time. 101 (pore diameter 50μm, thickness 3mm).

[0090] (2) Activated alumina: bake alumina with a particle size of 200 μm in a muffle furnace at 600° C. for 6 hours, and put it in a desiccator for use.

[0091] (3) Activated silica gel: bake silica gel with a particle size of 200 μm in a muffle furnace at 600° C. for 6 hours, take it out after cooling, and put it in a desiccator for later use.

[0092] (4) Preparation of silver nitrate-stained silica gel: Accurately weigh analytically pure silver nitrate in a volumetric flask, dissolve it with distilled wat...

Embodiment 3

[0096] Prepare the solid phase extraction column 1000 (such as Figure 16 shown):

[0097] (1) Prepare a 75mL glass chromatography column (i.e. hollow glass column 100). The bottom of the column tube is provided with an outlet of the extraction column, and a glass fiber sieve plate 101 is sintered close to the bottom of the column, and a glass fiber upper sieve plate matching the glass column is processed at the same time. 101 (pore size 30μm, thickness 2mm).

[0098] (2) Activated alumina: bake alumina with a particle size of 130 μm in a muffle furnace at 550° C. for 5 hours, and put it in a desiccator for use.

[0099] (3) Activated silica gel: bake silica gel with a particle size of 130 μm in a muffle furnace at 550° C. for 5 hours, take it out after cooling, and put it in a desiccator for later use.

[0100] (4) Preparation of silver nitrate-stained silica gel: Accurately weigh analytically pure silver nitrate in a volumetric flask, dissolve it with distilled water and c...

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Abstract

The invention discloses a solid-phase extraction column used cooperatively with a GC-FID instrument and application thereof. The solid-phase extraction column used cooperatively with the GC-FID instrument is applied to pretreatment of a to-be-detected sample for mineral oil contaminant detection of food. The solid-phase extraction column comprises a hollow glass column and a plurality of glass fiber sieve plates which are arranged in the hollow glass column and isolate the interior of the hollow glass column into a silver nitrate impregnated silica gel filling space used for filling of silver nitrate impregnated silica gel, an anhydrous sodium sulfate filling space used for filling of anhydrous sodium sulfate and an alumina filling space used for filling of alumina, wherein the silver nitrate impregnated silica gel filling space, the anhydrous sodium sulfate filling space and the alumina filling space are successively arranged from top to bottom. Through pretreatment of the sample for analysis of mineral oil contamination of food by using the solid-phase extraction column, analysis pollution can be effectively reduced, and repeatability and accuracy of sample detection are improved; and the solid-phase extraction column is applicable to most food.

Description

technical field [0001] The invention relates to a solid phase extraction column used in conjunction with a GC-FID instrument and applications thereof, in particular to a solid phase extraction column used in conjunction with a GC-FID instrument, and pretreatment of samples to be tested for detection of food mineral oil pollutants A method for detecting mineral oil contamination in food, a system for detecting mineral oil contamination in food, and a method for detecting mineral oil contamination in food. Background technique [0002] In recent years, the contamination of mineral oil in food has attracted much attention, mainly due to the migration of residual ink in recycled packaging paper. In addition, lubricants in plastic packaging (such as polystyrene, polyolefin), adhesives in waxed paper and hemp fiber packaging, mineral oil and white oil involved in food processing, and food raw materials during harvesting, drying and processing Mineral oil contamination of food can...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N1/34
CPCG01N1/34G01N30/02G01N2030/025G01N2030/027
Inventor 武彦文李冰宁刘玲玲黄华欧阳杰汪雨王欣欣
Owner BEIJING CENT FOR PHYSICAL & CHEM ANALYSIS
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