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Efficient capillary electrophoresis method for simultaneously detecting 11 prohibited compounds in sample

A technology for capillary electrophoresis and sample detection, which is applied in the field of chemical detection to achieve the effects of low analysis cost, good separation and reproducibility, and high separation.

Active Publication Date: 2015-05-06
康正检测服务股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

But for the metabolites of nitrofuran drugs, only AOZ and AMOZ can be measured, and positive samples need to be confirmed

Method used

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  • Efficient capillary electrophoresis method for simultaneously detecting 11 prohibited compounds in sample
  • Efficient capillary electrophoresis method for simultaneously detecting 11 prohibited compounds in sample
  • Efficient capillary electrophoresis method for simultaneously detecting 11 prohibited compounds in sample

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0057] 1、 Establishment of comparative electrophoresis spectra of standard substances of 11 prohibited compounds such as furazolidone

[0058] (1) Firstly prepare 1 mg / mL standard stock solutions of 11 prohibited compounds for use;

[0059] (2) Take 150 μL of AOZ, AMOZ, SEM, and AHD stock solutions, 150 μL of 50 mmol / L 2-NBA, 0.9 mL of 12 mol / L hydrochloric acid, and dilute to 10 mL with ultrapure water, and derivatize at 70 °C for 1 h;

[0060] (3) Adjust the pH of the derivative solution to 7.4 with 5 mol / L sodium hydroxide;

[0061] (4) Add 300 μL each of furazolidone, furaltadone, nitrofurazone, nitrofurantoin, nifursol, chloramphenicol and ciprofloxacin stock solutions;

[0062] (5) Inject samples under the above electrophoresis conditions to obtain the control electrophoresis spectra of 11 kinds of prohibited compounds such as furazolidone (see figure 1 ).

[0063] 2. Detection limits and concentrations of 11 prohibited compounds including furazolidone (Table 1)

...

Embodiment 2

[0074] Yellow bone fish sample detection:

[0075] (1) Preparation of homogeneous extract of yellow-bone fish: Weigh 100 g of homogeneous aquatic product (yellow-bone fish), put it in a 250 mL beaker, extract it ultrasonically with 150 mL of absolute ethanol for 30 min, and then add 80 mL of anhydrous Ethanol, repeated extraction 3 times, combined extracts, centrifuged at 3000 r / min for 10 min, poured the supernatant extract into a round-bottomed flask, concentrated under reduced pressure at 50 °C to nearly dryness, dissolved in 30 mL of acetonitrile and transferred to Add 10 mL of n-hexane to the separatory funnel, extract and separate, discard the n-hexane layer, repeat 5 times, pour the acetonitrile layer into a round-bottomed flask, concentrate under reduced pressure at 50 °C to nearly dryness, dissolve and transfer with absolute ethanol Put it into a graduated test tube, dry it with nitrogen at 50°C, dissolve it with acetonitrile-water (30:70) and dilute to 1 mL.

[0076...

Embodiment 3

[0079] Shrimp sample testing:

[0080] (1) Preparation of shrimp extract: 100 g of homogeneous aquatic product (shrimp) was weighed, placed in a 250 mL beaker, 150 mL of absolute ethanol was ultrasonically extracted for 30 min, 80 mL of absolute ethanol was added again, and the extraction was repeated 3 times. Combine the extracts, centrifuge at 3000 r / min for 10 min, pour the supernatant extract into a round-bottomed flask, concentrate under reduced pressure at 50 °C to nearly dryness, dissolve with 30 mL of acetonitrile and transfer to a separatory funnel, add 10 mL of n-hexane, extracted and separated, discarded the n-hexane layer, repeated 5 times, poured the acetonitrile layer into a round bottom flask, concentrated under reduced pressure at 50 ℃ to near dryness, dissolved with absolute ethanol and transferred to a graduated test tube, at 50 ℃ Blow dry under nitrogen gas, dissolve with acetonitrile-water (30:70) and dilute to 1 mL.

[0081] (2) Shrimp blank sample detect...

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Abstract

The invention discloses an efficient capillary electrophoresis method for simultaneously detecting 11 prohibited compounds in a sample. Metabolites are subjected to ultraviolet derivation by using 2-nitrobenzaldehyde (2-NBA), and then, the residues of the 11 prohibited compounds in an edible animal sample are simultaneously detected by using the efficient capillary electrophoresis method. The method is not only high in sensitivity, good in separation degree and repeatability, but also simple in sample pretreatment method, free of a large deal of organic solvent, low in analysis cost and suitable for microanalysis of residues of relevant prohibited compounds in the edible animal sample.

Description

technical field [0001] The invention belongs to the field of chemical detection, and in particular relates to a high-efficiency capillary electrophoresis method for simultaneously detecting 11 prohibited compounds in a sample. Background technique [0002] Furazolidone, furaltadone, nitrofurazone, nitrofurantoin, nifursol, chloramphenicol, and ciprofloxacin belong to broad-spectrum antibacterial drugs. These drugs are not only cheap and efficient, but also have killing effects on a variety of bacteria, so they are often used Farmers use it to raise edible animals such as aquatic products to prevent and treat common infectious diseases such as diarrhea and cholera. Some residues of these antibacterial drugs are extremely harmful to human health, and even have teratogenic and carcinogenic side effects. [0003] In fact, the half-life of nitrofuran drugs in animals is very short, mainly their metabolites 3-amino-2-oxazolidinone (AOZ), 5-methylmorpholine-3-amino-2-oxazolidine ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N27/447G01N1/28
Inventor 潘育方翟海云张兰春
Owner 康正检测服务股份有限公司
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