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

A solid-phase extraction column, basic dye technology, applied in the direction of material separation, analysis materials, instruments, etc., can solve the problems such as the lack of a variety of basic dye pretreatment and detection methods, tedious pretreatment work, etc. Stability and repeatability, shortened pre-processing time, fast effect

Active Publication Date: 2022-07-22
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 packing for basic dyes in food, solid-phase extraction column
  • Preparation method and application of solid-phase extraction packing for basic dyes in food, solid-phase extraction column
  • Preparation method and application of solid-phase extraction packing for basic dyes in food, solid-phase extraction column

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0072] Preparation of solid phase extraction packing: 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 respectively. 80.0 g of the powder was placed in a watch glass, ultrasonically reacted for 1 hour and then placed overnight, and vacuum-dried at 60°C for 12 hours to obtain a loose white powdery solid, which was a solid phase extraction filler.

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

[0074] The application of the above-mentioned solid phase extraction column in the rapid determination of the content of basic dyes in food by high performance liquid chromatography, its operation comprises the following steps:

[0075] Extraction of basic dyes: W...

Embodiment 2

[0081] Preparation of solid phase extraction packing: 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 respectively. 120.0 g of the powder was placed in a watch glass, ultrasonically reacted for 1 h and then placed overnight, and vacuum-dried at 70 °C for 15 h 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 other operations are the same as in Example 1.

[0083] The application of the above-mentioned solid phase extraction column in the rapid determination of the content of basic dyes in food by high performance liquid chromatography, its operation comprises the following steps:

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

Embodiment 3

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

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

[0092] The application of the above-mentioned solid phase extraction column in the rapid determination of the content of basic dyes in food by high performance liquid chromatography, its operation comprises the following steps:

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

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Abstract

The invention provides a preparation method and application of a solid-phase extraction filler and a solid-phase extraction column for basic dyes in food. Among them, the solid phase extraction fillers use functional ionic liquids 1-benzyl-3-methylimidazolium hexafluorophosphate and 1-decyl-3-methylimidazolium hexafluorophosphate, which are very similar in structure to basic dyes, as the main adsorption The reagent has strong specific adsorption capacity for various basic dyes, and does not adsorb impurities such as salts, sugars, pigments, oils, proteins, and starches in food matrices, and can effectively separate impurities and alkalis in the sample to be tested. Sex dyes. In addition, silica gel is used to immobilize the functional ionic liquid to form a loose solid-phase extraction filler, which can also be fully contacted with the extraction liquid of the sample to be tested without extrusion. The sample liquid passes through the packing quickly, which improves the extraction efficiency and shortens the sample pretreatment time. The solid phase extraction column made of the filler can be used for the rapid determination of the basic dye content in food 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 solid-phase extraction packing of basic dyes in food and a solid-phase extraction column. Application in the rapid determination of sex dye content. Background technique [0002] Basic dyes are salts of aromatic bases and organic or inorganic acids, that is, salts of colored organic bases. Its basic group is generally amino, and it is -NH after salt formation. 2 • HCl salt group. [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 Rhodane appeared one after another. Ming (C.I. Basic Violet 10) and many other varieties. The chemical structure of basic dyes includes diarylmethane, triarylmethane, azo type and nitrogen-cont...

Claims

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Application Information

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Patent Type & Authority Patents(China)
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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