Extraction head for solid phase micro-extraction, and preparation method and applications of extraction head

An extraction head and extraction technology, applied in separation methods, chemical instruments and methods, and other chemical processes, can solve problems such as poor stability and specificity, matrix and environmental interference, and short service life, and achieve good stability and improved The effect of mechanical strength and easy operation

Inactive Publication Date: 2013-01-02
XIAMEN UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The purpose of the present invention is to provide a simple preparation method, low cost, and high extraction capacity for aldehydes produced by oxidation of oils, aiming at the shortcomings of existing commercial extraction heads such as low mechanical strength and short service life. A solid-phase microextraction head that overcomes the fragility of quartz fibers, good practical value, stable physical and chemical properties, and ease of popularization and use, as well as its preparation method and application
[0005] Another object of the present invention is to provide a method that can overcome the existing thiobarbituric acid reaction product value method that is susceptible to substrate and environmental interference, An extraction and analysis method based on a new solid-phase microextraction coating with the disadvantages of poor stability and specificity

Method used

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  • Extraction head for solid phase micro-extraction, and preparation method and applications of extraction head
  • Extraction head for solid phase micro-extraction, and preparation method and applications of extraction head
  • Extraction head for solid phase micro-extraction, and preparation method and applications of extraction head

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Effect test

Embodiment 1

[0040] Example 1: ZnO nanorod coatings were directly prepared on modified stainless steel wire substrates by hydrothermal synthesis. Before the preparation, the stainless steel substrate was ultrasonically cleaned with acetone and water for 5 min, and then dried naturally at room temperature. Prepare zinc oxide reaction solution: add 20mL deionized water to a 25mL reaction bottle, then add equimolar zinc nitrate hexahydrate and hexamethylenetetramine to the solution to obtain 0.025mol L -1 The reaction solution was homogeneously mixed by ultrasonication. Pass the cleaned stainless steel substrate through the self-made foam bottle cap, and directly immerse it vertically in the reaction solution. Leave about 1 cm of stainless steel wire in the reaction bottle to grow the coating, and seal the reaction bottle. The reaction vial was placed in an oven at 90 °C for 4 h. After the reaction was completed, the stainless steel wire fiber was taken out, and the zinc oxide nanorod layer...

Embodiment 2

[0041] Example 2: The following is a comparison of the extraction efficiency of the zinc oxide nanorod coating prepared by the present invention for 5 kinds of aldehyde compounds with that of a commercial extraction head. Depend on image 3 It can be seen that for most of the target aldehydes, the ZnO nano-coating has comparable extraction efficiency to the commercial coating. The thickness of the zinc oxide nano-coating is only 5 μm, while the thickness of the commercial coating is 85 μm. Since zinc oxide nanorods have a large specific surface area and a certain polar surface, it has a high extraction efficiency for volatile aldehydes. This more regular arrangement of ZnO nanorods increases the effective surface area and thus increases the extraction sites of the fibers accordingly. This solid-phase microextraction method based on zinc oxide nanorod coating has a good extraction effect for aldehydes produced by oxidation in complex food matrices.

[0042] GC / FID operating ...

Embodiment 3

[0043] Example 3: The detection results of target aldehydes in three actual instant noodle samples by the solid-phase microextraction-gas chromatography method based on zinc oxide nanorod coating established in the present invention are given below. Table 1 shows that this method can detect the target aldehyde compounds in instant noodle samples, and has a good recovery rate, the recovery rate ranges from 70.5% to 129.4%.

[0044] Table 1

[0045]

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Abstract

The invention provides an extraction head for solid phase micro-extraction, a preparation method of the extraction head and applications of the extraction head, and relates to solid phase micro-extraction. The extraction head is provided with a stainless steel substrate which is a stainless steel fiber, wherein one end of the stainless steel fiber is provided with a section of stainless steel hollow conduit and the tail end of the stainless steel fiber is provided with a zinc oxide nanorod coat. The preparation method comprises the following steps: fixing one section of stainless steel hollow conduit on the bottom end of the substrate, wherein the stainless steel hollow conduit enables one end of the coat which is close to the stainless steel hollow conduit to be always in the center of a needle tubing; preparing a zinc oxide reaction solution; adding zinc nitrate hexahydrate and hexamethylenetetramine to obtain a reaction solution; immersing the substrate in the reaction solution; reserving1-2cm stainless steel wire in a reaction bottle in order to grow the coat; sealing the reaction bottle; taking out the stainless steel wire after the reaction is finished; washing the zinc oxide nanorod coat; removing residuals from the surface and drying; and then assembling the prepared zinc oxide nanorod fiber with a 5muL micro-feeder to obtain a solid phase micro-extraction device.

Description

technical field [0001] The invention relates to a solid-phase microextraction, in particular to an extraction and analysis detection method of a new solid-phase microextraction coating used for oil oxidation detection in oily food. Background technique [0002] Dietary lipids are one of the essential nutrients for the human body and play an important role in the nutritional composition of the human body. Dietary lipids can not only supply calories and essential fatty acids to the human body, but also serve as carriers of fat-soluble vitamins to increase the flavor of food. However, foods containing dietary lipids are easily oxidized during processing, transportation, and storage. In addition to great changes in taste, flavor, and color, the oxidized foods will also undergo some oxidation. Hazard to human health. Oxidized oils can cause systemic toxicity, neurotoxicity, cytotoxicity, and genotoxicity. Therefore, it is very necessary to develop a method that can accurately ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J20/281B01J20/32B01J20/06B01D15/08B01D15/20G01N30/06
Inventor 陈曦姬姣姣王翊如何春燕屈艳勤
Owner XIAMEN UNIV
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