A shell-core magnetic microsphere and its extraction method for clenbuterol in mutton

A nuclear structure, clenbuterol technology, applied in chemical instruments and methods, sampling, other chemical processes, etc., can solve the problems of large consumption of organic solvents, only one use, and low specificity, and achieve clear chromatographic peaks. , the effect of less interference and improved sensitivity

Active Publication Date: 2021-08-03
JILIN INST OF CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Due to the problems of large consumption of organic solvents, low specificity, high price, and only one-time use of traditional solid-phase extraction small columns, it is necessary to develop a solid-phase extraction column with strong enrichment ability for clenbuterol, simple preparation method, low price, and Selective new extraction material

Method used

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  • A shell-core magnetic microsphere and its extraction method for clenbuterol in mutton
  • A shell-core magnetic microsphere and its extraction method for clenbuterol in mutton
  • A shell-core magnetic microsphere and its extraction method for clenbuterol in mutton

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Experimental program
Comparison scheme
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Embodiment 1

[0036] The present embodiment provides a kind of shell-core structure magnetic nano-microsphere and preparation method thereof, and the magnetic Fe of 0.2g is weighed 3 o 4 @C, add 11.6mL of ultrapure water, 8.3mL of absolute ethanol, 0.1mL of butanol, 0.291g of cobalt nitrate (1mmoL), 0.1g of sodium citrate (Na 3 Cit) and 0.16 g of urea, ultrasonically until uniformly mixed, the mixture was transferred to a 50 mL hydrothermal synthesis kettle, placed in an oven and heated to 120°C. After 8 hours of reaction, the magnetic Fe 3 o 4 @C@Co 3 o 4 Separated by a magnet, washed thoroughly with ultrapure water and absolute ethanol, and dried in a vacuum oven at 60°C.

[0037] In the following, the magnetic Fe is characterized by methods such as infrared spectroscopy, X-ray diffraction (XRD), and transmission electron microscopy (TEM). 3 o 4 @C@Co 3 o 4 physical and chemical properties.

[0038] Depend on figure 1 It can be seen that, as shown in a, Fe can be observed 3 o ...

Embodiment 2

[0042] This embodiment utilizes the shell-core structure magnetic nano-microspheres Fe prepared in Example 1 3 o 4 @C@Co 3 o 4 The method for extracting clenbuterol in mutton comprises the following steps:

[0043] Use 30mL of absolute ethanol to ultrasonically extract the clenbuterol in 10g of mutton to obtain a sample solution containing clenbuterol, blow it dry with nitrogen, adjust the volume to 50mL with ultrapure water, and adjust the pH to 9 with hydrochloric acid or sodium hydroxide solution to obtain Extraction solution;

[0044] Get above-mentioned extraction solution 10mL, then add described magnetic adsorbent Fe 3 o 4 @C@Co 3 o 4 20mg, vortex extraction for 20min, magnetically separate the adsorbent loaded with clenbuterol, discard the supernatant; add eluent acetic acid: methanol = 15%: 85% eluent 3mL, vortex again for 10min, magnetic Separate, pipette the supernatant and dry it under nitrogen in a water bath, dilute to 1 mL with ultrapure water, and perf...

Embodiment 3

[0046] Investigating magnetic microspheres Fe 3 o 4 @C@Co 3 o 4 The effect of dosage on the extraction efficiency of clenbuterol from mutton.

[0047] Clenbuterol in mutton is extracted according to the method described in Example 2, the difference is that the magnetic microsphere Fe 3 o 4 @C@Co 3 o 4 The added amount of the drug was 5, 10, 15, 20, 30mg respectively. Such as Figure 4 As shown, in the magnetic microsphere Fe 3 o 4 @C@Co 3 o 4 When the mass is 20 mg, the extraction efficiency of the three is better, therefore, the optimum adsorbent mass selected by the present invention is 20 mg.

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Abstract

The invention discloses a magnetic nano-microsphere with a shell-core structure and a method for extracting clenbuterol from mutton, wherein the magnetic nano-microsphere is Fe 3 o 4 @C@Co 3 o 4 , the present invention is based on the magnetic solid-phase extraction technology, using the magnetic nano-microspheres as the adsorbent to extract the clenbuterol in the mutton, and realizes the selective enrichment of the clenbuterol in the mutton sample to be tested, It can significantly improve the sensitivity of high performance liquid chromatography (equipped with ultraviolet detector) to detect clenbuterol in mutton.

Description

technical field [0001] The invention belongs to the technical field of food detection, and in particular relates to a magnetic microsphere with a shell-core structure and a method for extracting clenbuterol from mutton. Background technique [0002] In recent years, reports of detection of clenbuterol in some pigs, sheep, beef and other meats have occurred frequently, and the common people are paying more and more attention to the hygienic production conditions of some meats and their meat products. Clenbuterol is a feed additive that can cause serious adverse reactions to the human body. If people eat a large amount of meat products that exceed the standard, they will be poisoned and even die. How to quickly and effectively detect the content of clenbuterol in meat has become a common concern. [0003] Since the meat matrix is ​​complex and the content of clenbuterol is usually trace level, pretreatment of the sample is required. Due to the problems of large consumption o...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J20/281B01J20/28B01J20/30G01N1/34G01N1/40
CPCB01J20/28007B01J20/28009B01J20/28019B01J20/281G01N1/34G01N1/4044G01N1/405G01N1/4055G01N1/4077G01N2001/4061
Inventor 连丽丽张鑫洋娄大伟王希越李玉莹吕进义
Owner JILIN INST OF CHEM TECH
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