Preparation method of freeze-dried powder standard sample of animal-sourced substrate drug and metabolite residue thereof

A standard sample, animal-derived technology, applied in the preparation of test samples, etc., can solve the problems of unconvincing test results, high price, transportation problems, etc., achieve significant economic value and market competitiveness, and uniform and stable samples , use reliable effects

Inactive Publication Date: 2014-11-19
威海出入境检验检疫局检验检疫技术中心 +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, domestic residue analysis laboratories often cannot obtain actual contaminated samples, so they often add veterinary drug standard solutions to the analysis samples for quality control, which cannot truly reproduce the extraction efficiency of drugs in animals after natural metabolism, and cannot reflect the method. Accuracy, the test results obtained are not convincing enough
The European Union’s regulations on veterinary drug residue analysis methods and result expression 2002 / 657 / EC clearly pointed out the need to use standard samples for process control. Foreign residue analysis laboratories have generally used standard sample samples for laboratory quality control and result evaluation, mainly by Provided by the Institute of Standard Materials and Measurement (IRMM) of the European Community and FAPAS of the United Kingdom, relevant samples have also been industrialized, but due to the high price of foreign standard samples or quality control samples, and the need for transportation Problem, domestic residue analysis laboratories cannot regularly use it for quality control

Method used

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  • Preparation method of freeze-dried powder standard sample of animal-sourced substrate drug and metabolite residue thereof
  • Preparation method of freeze-dried powder standard sample of animal-sourced substrate drug and metabolite residue thereof
  • Preparation method of freeze-dried powder standard sample of animal-sourced substrate drug and metabolite residue thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] Example 1, a method for preparing a standard sample of toltrazuril and its metabolite toltrazuril sulfone residual freeze-dried powder in chicken, this example takes the control target content level of 20-100ug / kg as an example, and its specific steps as follows:

[0018] (1) Selection of experimental animals: Broiler chickens purchased from the market are required to be of uniform size and average weight of 2.2-2.7 kg. First, confirm that the broiler chickens have not been fed with toltrazuril, randomly sample them, and feed them after the test confirms that the samples are negative. After 5 days of normal feeding, the injured and unhealthy chickens were removed.

[0019] (2) Feeding with drugs: Accurately weigh 0.2 mg of toltrazuril powder, put it into capsules, feed each chicken with 1 capsule per day, and feed it for 2 consecutive days, slaughter it 10 hours after stopping the drug on the second day, and take the breast muscle Detection, at this time the concentrat...

Embodiment 2

[0079] A method for preparing a standard sample of florfenicol residual freeze-dried powder in shrimp meat. This embodiment takes the control target content level of 1-100ug / kg as an example, and its specific steps are as follows:

[0080] (1) Selection of experimental animals: Live vannamei shrimp purchased from the market require uniform size and an average weight of about 20-30 g. First, confirm that the live shrimp has not been fed Florfenicol. Random sampling is carried out, and the test confirms that it is a negative sample . After 2 days of normal breeding, remove the injured and unhealthy shrimp.

[0081] (2) Drug feeding: Accurately weigh the florfenicol powder, add the drug at a concentration of 0.5 mg / L in the pool water, administer the drug in the whole pool in a splash-type dipping bath, change the water once a day, and remove the shrimp 8 hours after the drug on the second day. Take them all out, wash them with clean water, peel off the skin and get the shrimp m...

Embodiment 3

[0137] A method for preparing a standard sample of freeze-dried powder of three β-stimulant residues in beef, using clenbuterol, salbutamol and ractopamine standard preparation solution to intramuscularly inject cattle and control the slaughter time, so that the cattle contain the above three The drug is basically uniform, slaughtered and homogenized from beef muscle to make minced meat, freeze-dried, degreased, sieved, bottled, and vacuum-packaged to prepare a standard sample containing three β-stimulant residues in beef muscle powder. In this embodiment, the control target content level of 1-10ug / kg is taken as an example, and the specific steps are as follows:

[0138] (1) Selection of experimental animals: Select healthy cows with a weight of about 60-100kg. The feeding of the cows should be controlled 7 days before the injection, and the use of other drugs is prohibited, so that the drugs that may remain in the cows can be completely metabolized out of the body.

[0139] ...

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Abstract

The invention provides a preparation method of a freeze-dried powder standard sample of an animal-sourced substrate drug and a metabolite residue thereof. The method includes following steps: feeding experimental animals with drugs, wherein a drug feeding method is feeding, injecting or medicated bath with one or more drugs; controlling a feeding time; obtain a sample material containing raw drugs and/or metabolites through metabolism in animal bodies; adding a vitamin C solution; performing a mashing and homogenizing process to obtain meat paste; performing a vacuum freeze-drying process, a crushing and sieving process and a nitrogen-filling package process and a vacuum packaging process. In addition, a degreasing, repeated homogenizing and sieving process is included or not included according to fat content in an animal substrate. The standard sample can be transported at normal temperature and is long in preserving time. A situation of combination of a target object and the substrate is coincided with that of an actual detection sample. The standard sample can be used of quality controlling of relative detection and analysis, is homogeneous and stable, is convenient to transport, is reliable in use and has significant economic value and market competitiveness.

Description

technical field [0001] The invention belongs to the technical field of animal source matrix standard samples for detection of drug residues, specifically a method for raising animals with common veterinary drugs to obtain animal matrix with a considerable drug concentration, and vacuum freeze-drying to form freeze-dried powder standard samples. Background technique [0002] Typical veterinary drugs refer to drugs used to prevent and treat livestock and poultry diseases. However, with the development of intensive breeding production, some chemical and biological medicinal ingredients have been developed into animal health products or feed additives with certain functions, which also belong to the category of veterinary drugs. The main uses of veterinary drugs are to prevent and treat diseases, promote growth, improve production performance, and improve the quality of animal food. Veterinary drug residues refer to the accumulation and storage of the original compounds of vete...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N1/28G01N1/42
Inventor 杨丽君王静胡巧茹刘玉敏李兆杰梁君妮王美玲宋晓华
Owner 威海出入境检验检疫局检验检疫技术中心
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