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A kind of detection method of quinolones in feed

A technology of quinolones and detection methods, which is applied in the field of feed detection, can solve the problems of insufficient sensitivity and accuracy, and cannot meet the detection requirements of quinolones, and achieve improved sensitivity and accuracy, good selectivity and sensitivity, and accurate qualitative improvement effect of ability

Active Publication Date: 2022-05-27
浙江国正检测技术有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The purpose of the present invention is to overcome the problem that the detection method of quinolones in the prior art is still insufficient in sensitivity and accuracy, and cannot meet the feed detection requirements of complex matrix components and low content of quinolones to be tested, and provides a A method for the detection of quinolones in feed, using ultra-high pressure liquid chromatography-quadrupole / electrostatic field orbitrap high-resolution mass spectrometry for the determination of quinolones in feed, simple operation, accurate qualitative and quantitative analysis, realized Sensitive, rapid and accurate determination of quinolones in feed

Method used

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  • A kind of detection method of quinolones in feed
  • A kind of detection method of quinolones in feed
  • A kind of detection method of quinolones in feed

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0056] Sample pretreatment method: Weigh 2.00 g of the feed to be tested (crushed through a 100-mesh sieve) into a 10 mL centrifuge tube, add 20 mL of acetonitrile-water solution (4:1, V / V) containing 0.1 wt% formic acid, and vortex mix , shake and extract for 10 min, take 1 mL of the supernatant, dilute to 10 mL with 10 wt % acetonitrile aqueous solution, centrifuge for 15 min, the supernatant is the extract, and carry out solid-phase extraction on the molecularly imprinted monolithic column on the extract, the extraction method is as follows:

[0057] Activate the molecularly imprinted monolithic column with methanol and water at a flow rate of 0.75mL / min for 4min, take 1mL of the extract and load the sample, rinse the column with water at a flow rate of 0.75mL / min for 4min, and then use a volume ratio of 1.5:1 The methanol / acetic acid eluent was eluted for 8 minutes, and the eluate was collected. After blowing dry with nitrogen at 45°C, the residue was dissolved in 1 mL of 0...

Embodiment 2

[0066] Sample pretreatment method: Weigh 1.00 g of the feed to be tested (crushed through a 100-mesh sieve) into a 10 mL centrifuge tube, add 15 mL of acetonitrile-water solution (5:1, V / V) containing 0.15 wt% formic acid, and vortex mix , shake and extract for 12 minutes, take 1 mL of the supernatant, dilute to 10 mL with 10wt% acetonitrile aqueous solution, and centrifuge for 12 minutes.

[0067] Activate the molecularly imprinted monolithic column with methanol and water at a flow rate of 0.5mL / min in sequence for 6min, take 1mL of the extract and load the sample, rinse the column with water at a flow rate of 0.5mL / min for 6min, and then use a volume ratio of 1:1 The methanol / acetic acid eluent was eluted for 10 minutes, and the eluate was collected. After drying with nitrogen at 40°C, the residue was dissolved in 0.5 mL of 0.15 wt% formic acid acetonitrile solution, and passed through a 0.22 μm filter membrane to obtain the pretreated sample;

[0068] The preparation meth...

Embodiment 3

[0076] Sample pretreatment method: Weigh 2.00 g of the feed to be tested (crushed through a 100-mesh sieve) into a 10 mL centrifuge tube, add 20 mL of acetonitrile-water solution (4:1, V / V) containing 0.15 wt% formic acid, and vortex mix , shake and extract for 15 minutes, take 1 mL of the supernatant, dilute to 10 mL with 10 wt% acetonitrile aqueous solution, centrifuge for 15 minutes, the supernatant is the extract, and carry out solid-phase extraction on the molecularly imprinted monolithic column on the extract, the extraction method is as follows:

[0077] Activate the molecularly imprinted monolithic column with methanol and water respectively at a flow rate of 1.0mL / min for 3min, take 0.5mL of the extract and load the sample, rinse the column with water at a flow rate of 1.0mL / min for 3min, and then use a volume ratio of 1: 1 methanol / acetic acid eluent was eluted for 5 minutes, the eluate was collected, and after being blown dry with nitrogen at 50°C, the residue was di...

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Abstract

The invention discloses a method for detecting quinolones in feed. The steps are: (1) using an ultra-high pressure liquid chromatography-quadrupole / electrostatic field orbitrap high-resolution mass spectrometer to measure the accurate mass database of the quinolones to be tested and mass spectral library; (2) extract the feed with formic acid acetonitrile solution, and the extract is subjected to molecular imprinted monolithic column solid-phase extraction and elution to obtain the pretreated sample; (3) sample detection; (4) sample detection results Perform comparative analysis with the established accurate mass database and mass spectral library, and when the detection result completely matches the information of the accurate mass database and mass spectral library, it is determined that the quinolones to be tested are detected in the sample. The invention adopts ultra-high pressure liquid chromatography-quadrupole / electrostatic field orbitrap high-resolution mass spectrometry to measure the quinolones in the feed, the operation is simple, the qualitative and quantitative analysis is accurate, and the sensitivity to the quinolones in the feed is realized. , Rapid and accurate determination.

Description

technical field [0001] The invention relates to the technical field of feed detection, in particular to a detection method for quinolones in feed. Background technique [0002] Quinolones are a class of artificially synthesized drugs with antibacterial effects. They have the characteristics of broad antibacterial spectrum, strong antibacterial power, small toxic and side effects, and low price. They are widely used in aquaculture as feed additives to prevent and treat livestock and poultry disease. Bacterial infectious diseases of fish. Due to insufficient understanding of drug knowledge, and even driven by economic interests, it is not uncommon for non-standard drug use, abuse of veterinary drugs, and illegal addition of drugs to feed. Drugs in the feed are excreted through excrement through animal metabolism or directly enter the water body and remain in the soil, water body, and plants. In addition, quinolones themselves have certain toxicity, and their potential carcino...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/88G01N30/06G01N30/72B01J20/281B01J20/26
CPCG01N30/88G01N30/06G01N30/72B01J20/281B01J20/268G01N2030/884G01N2030/062
Inventor 汪行舟代兵李华何艳吕凯凯
Owner 浙江国正检测技术有限公司
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