Preparation method and application of solid-phase extraction filler and solid-phase extraction column for basic dyes in food

A solid-phase extraction column, basic dye technology, applied in the direction of material separation, analysis materials, instruments, etc., can solve the problems of tedious pretreatment work, there are no various basic dye pretreatment and detection methods, etc., to shorten the sample Pretreatment time, favorable for stability and repeatability, and low reagent cost

Active Publication Date: 2020-03-31
嘉峪关市食品药品和医疗器械检验检测中心
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, this method requires cumbersome pretreatment of samples during the actual operation, and food is a complex matrix sample containing a variety of basic dyes. At present, there is no pretreatment and detection method for various basic dyes in this complex matrix sample.

Method used

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  • Preparation method and application of solid-phase extraction filler and solid-phase extraction column for basic dyes in food
  • Preparation method and application of solid-phase extraction filler and solid-phase extraction column for basic dyes in food
  • Preparation method and application of solid-phase extraction filler and solid-phase extraction column for basic dyes in food

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0072] Preparation of solid-phase extraction filler: Weigh 10.0 g of 1-benzyl-3-methylimidazolium hexafluorophosphate, 40.0 g of 1-decyl-3-methylimidazolium hexafluorophosphate, 200 g of methanol, and 100 mesh silica gel 80.0 g of the powder was placed in a watch glass, ultrasonically reacted for 1 hour, left overnight, and then vacuum-dried at 60°C for 12 hours to obtain a loose white powdery solid, which was the solid-phase extraction filler.

[0073] Preparation of solid-phase extraction column: Weigh 400 mg of the above-mentioned solid-phase extraction filler, place it in a sleeve, compress the filler, cover with fiberboard and plastic cover in turn, and finally put on a pressure-resistant ring.

[0074] The above-mentioned solid-phase extraction column is used in the rapid determination of basic dye content in food by high-performance liquid chromatography, and its operation includes the following steps:

[0075] Extraction of basic dyes: Weigh 2.00g of chili oil into a 1...

Embodiment 2

[0081] Preparation of solid-phase extraction filler: Weigh 20.0 g of 1-benzyl-3-methylimidazolium hexafluorophosphate, 50.0 g of 1-decyl-3-methylimidazolium hexafluorophosphate, 200 g of methanol, and 100 mesh silica gel 120.0 g of the powder was placed in a watch glass, ultrasonically reacted for 1 hour, left overnight, and then vacuum-dried at 70°C for 15 hours to obtain a loose white powdery solid, which was the solid-phase extraction filler.

[0082] Preparation of solid-phase extraction column: Weigh 600 mg of the above-mentioned solid-phase extraction filler, and the rest of the operations are the same as in Example 1.

[0083] The above-mentioned solid-phase extraction column is used in the rapid determination of basic dye content in food by high-performance liquid chromatography, and its operation includes the following steps:

[0084] Extraction of basic dyes: Weigh 2.00g of black wolfberry into a 15mL centrifuge tube, add 5mL of acetonitrile, 6mL of methanol, and 2mL...

Embodiment 3

[0090] The solid-phase extraction filler of this embodiment is prepared in this way: Weigh 30.0 g of 1-benzyl-3-methylimidazolium hexafluorophosphate, 60.0 g of 1-decyl-3-methylimidazolium hexafluorophosphate, methanol 200g, 100.0g of 100-mesh silica gel powder was placed in a glass beaker, ultrasonically reacted for 1h, then left overnight, and vacuum-dried at 75°C for 18h to obtain a loose white powdery solid, which was the solid-phase extraction filler.

[0091] Preparation of solid-phase extraction column: Weigh 500 mg of the above-mentioned solid-phase extraction filler, and the rest of the operations are the same as in Example 1.

[0092] The above-mentioned solid-phase extraction column is used in the rapid determination of basic dye content in food by high-performance liquid chromatography, and its operation includes the following steps:

[0093]Extraction of basic dyes: Weigh 2.00g of mulberry into a 15mL centrifuge tube, add 6mL of acetonitrile, 6mL of methanol, and ...

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Abstract

The invention provides a preparation method and application of solid-phase extraction filler and solid-phase extraction column for basic dyes in food. The solid-phase extraction filler adopts functional ionic liquid 1-benzyl-3-methylimidazolium hexafluorophosphate and 1-decyl-3-methylimidazolium hexafluorophosphate, which have structures extremely similar to those of basic dyes, as main adsorptionreagents; the specific adsorption capacity on various basic dyes is high, impurities such as salt, carbohydrate, pigment, grease, protein and starch in a food matrix are not adsorbed, and the impurities and the basic dyes in a to-be-detected sample can be effectively separated. The functional ionic liquid is immobilized by silica gel to form a loose solid-phase extraction filler, and the loose solid-phase extraction filler can be in full contact with an extracting solution of a to-be-detected sample without extrusion. The speed of the sample liquid passing through the filler is high, the extraction efficiency is improved, and the sample pretreatment time is shortened. A solid-phase extraction column prepared from the filler can be used for rapidly determining the content of basic dyes infood in high performance liquid chromatography, and the determination result is accurate and stable.

Description

technical field [0001] The invention belongs to the technical field of food safety detection, and relates to a preparation method of a basic dye solid-phase extraction filler in food and a solid-phase extraction column. Application in rapid determination of permanent dye content. Background technique [0002] Basic dyes are salts of aromatic bases and organic or inorganic acids, that is, colored salts of organic bases. Its basic group is generally amino, and it is -NH after salt formation 2 • HCl salt groups. [0003] In 1856, H.W.perkin synthesized the world's first synthetic dye aniline violet, which is a basic dye. After that, basic fuchsin (C.I. basic violet 14), basic blue (C.I basic blue 9), crystal violet (C.I basic violet 3), malachite green (C.I. basic green 4) and rhodan appeared successively. Ming (C.I. Basic Violet 10) and many other varieties. The chemical structure of basic dyes includes diaryl methane, triaryl methane, azo type and nitrogen-containing het...

Claims

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Application Information

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IPC IPC(8): G01N30/06G01N30/74
CPCG01N30/06G01N30/74
Inventor 沈海波张连钢周鑫魁刘燕珺方剑儒
Owner 嘉峪关市食品药品和医疗器械检验检测中心
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