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Method for determining antibiotic residues

A method of determination and antibiotic technology, applied in the direction of measuring devices, instruments, scientific instruments, etc., can solve the problems of high detection limit, difficult separation of oxytetracycline and chlortetracycline, etc., and achieve good separation effect

Active Publication Date: 2020-12-08
ZHEJIANG CENT FOR DISEASE CONTROL & PREVENTION
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] The object of the present invention is to provide a fast, sensitive, high accuracy, good separation effect, can simultaneously measure OTC, TC, CTC residual and be suitable for the method for the determination of three kinds of tetracycline antibiotic residues in animal food, which is suitable for large batch sample detection, It aims to solve the problems of difficult separation of oxytetracycline and aureomycin and high detection limit existing in the prior art

Method used

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  • Method for determining antibiotic residues
  • Method for determining antibiotic residues
  • Method for determining antibiotic residues

Examples

Experimental program
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Effect test

Embodiment 1

[0034] Accurately weigh 5g of chopped and homogenized animal food into a 50ml centrifuge tube, add 10ml of 5% perchloric acid solution, ultrasonically extract for 15min, draw the supernatant into another 50ml centrifuge tube, add 5% perchloric acid Repeat the extraction once with 10ml of acid solution, combine the two extracts, centrifuge at 3000r / min for 15min, after the temperature is less than 30°C, dry and concentrate with nitrogen, add divalent manganese ions to the extracted concentrated supernatant to obtain ions Liquid, apply a high-voltage pulse electric field to the ionic liquid, the high-voltage pulse electric field treatment conditions are field strength 20kv / cm, the number of pulses is 6, and the time is 5min. The high-voltage pulse electric field polarizes metal ions and tetracycline antibiotic molecules in the ionic liquid to achieve For the complex ionic liquid of metal ions and tetracycline antibiotic molecules, add 10ml EDTA-McIlvaine buffer solution for low-t...

Embodiment 2

[0036]Heat the animal food to 60°C, keep it for 5 minutes, then put it into a liquid nitrogen bucket, freeze-dry it with liquid nitrogen for 6-12 hours, the freezing temperature is lower than -30°C, and then crush it with a pulverizer until the particle size is less than 0.3mm. Take 1g of crushed material and add it to 10ml of acetonitrile with a pH value of 4.5 and mix well, put 5g into a 50ml centrifuge tube, add 10ml of 5% perchloric acid solution, ultrasonically extract for 15min, absorb the supernatant into another 50ml centrifuge tube , plus 10ml of 5% perchloric acid solution to repeat the extraction once, combine the 2 extracts, and centrifuge at a speed of 3000r / min for 15min. Add divalent manganese ions to obtain ionic liquid, and apply high-voltage pulse electric field to the ionic liquid. The high-voltage pulse electric field treatment conditions are field strength 20kv / cm, pulse number 6, and time 5min. Molecules undergo polarization to realize the complexation of...

Embodiment 3

[0038] Heat the animal food to 60°C, keep it for 5 minutes, then put it into a liquid nitrogen bucket, freeze-dry it with liquid nitrogen for 6-12 hours, the freezing temperature is lower than -30°C, and then crush it to a particle size of less than 0.3mm through a pulverizer. Take 1g of crushed material and add it to 10ml of acetonitrile with a pH value of 4.5 and mix well, put 5g into a 50ml centrifuge tube, add 10ml of 5% perchloric acid solution, ultrasonically extract for 15min, absorb the supernatant into another 50ml centrifuge tube , plus 10ml of 5% perchloric acid solution to repeat the extraction once, combine the 2 extracts, and centrifuge at a speed of 3000r / min for 15min. Add divalent manganese ions to obtain ionic liquid, and apply high-voltage pulse electric field to the ionic liquid. The high-voltage pulse electric field treatment conditions are field strength 20kv / cm, pulse number 6, and time 5min. Molecules undergo polarization to realize the complexation of ...

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Abstract

The invention relates to the technical field of antibiotic detection, and discloses a method for determining antibiotic residues, which comprises the following steps: heating a high-voltage pulsed electric field in sample pretreatment, and designing a crushing step, so that oxytetracycline, tetracycline and aureomycin have favorable peak shapes and are well separated within 10 minutes during detection; the linear relation is good, and the correlation coefficients are all 0.9992 or above; the RSD of oxytetracycline, tetracycline and aureomycin with three different standard concentrations is 5%or below, and the reproducibility is good; the adding standard recovery rate is greater than 85%; the detection limit of oxytetracycline is 3.3 * 10 <3> mu g / ml, the detection limit of tetracycline is3.8 * 10 <3> mu g / ml, the detection limit of aureomycin is 4.6 * 10 <3> mu g / ml, and the detection limit is relatively low; therefore, the method can satisfy simultaneous, rapid, accurate and large-batch detection of oxytetracycline, tetracycline and aureomycin.

Description

technical field [0001] The patent of the present invention relates to the technical field of antibiotic detection, in particular, to a method for determining antibiotic residues. Background technique [0002] Tetracyclines (TCs) are a class of broad-spectrum antibiotics, mainly including tetracycline (TC), chlortetracycline (CTC), oxytetracycline (Oxytetracycline, OTC), etc. It is widely used in poultry farming. If residents eat animal foods containing TCs antibiotics for a long time or in large quantities at one time, it will cause flora imbalance, gastrointestinal reactions, liver damage, and affect the development of teeth and bones. [0003] At present, the detection methods of tetracycline antibiotic residues mainly include microbiological method, immunoassay method, thin layer chromatography, capillary electrophoresis method, electrochemical method, high performance liquid chromatography and so on. At present, many high-performance liquid chromatography methods are u...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/06G01N30/86
CPCG01N30/02G01N30/06G01N30/8675G01N2030/062G01N2030/067
Inventor 曹艺耀汪倩王鹏任鸿汤鋆周振徐秋凉张美辨楼晓明张东霞
Owner ZHEJIANG CENT FOR DISEASE CONTROL & PREVENTION
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