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Choking-state and free-state coexisting ractopamine standard substance in swine urine matrix as well as preparation method and application of ractopamine standard substance

A technology for ractopamine and ractopamine pigs is applied in the field of preparation of veterinary drug residue detection standards, which can solve the problems affecting the accuracy, reliability and comparability of detection results, and achieve good uniformity and stability.

Active Publication Date: 2021-06-04
INST OF AGRO FOOD SCI & TECH CHINESE ACADEMY OF AGRI SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Therefore, the so-called positive samples of pig urine simulated to contain ractopamine obtained through "temporary preparation" will seriously affect the accuracy, reliability and comparability of the test results in the food safety monitoring work

Method used

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  • Choking-state and free-state coexisting ractopamine standard substance in swine urine matrix as well as preparation method and application of ractopamine standard substance
  • Choking-state and free-state coexisting ractopamine standard substance in swine urine matrix as well as preparation method and application of ractopamine standard substance
  • Choking-state and free-state coexisting ractopamine standard substance in swine urine matrix as well as preparation method and application of ractopamine standard substance

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] Example 1 Standard substance candidate preparation

[0028] In a pig farm with a scale of about 1000 pigs, 12 representative pigs during the fattening period (4-5 months old, 2-4 weeks before slaughter, weighing about 120kg) were randomly selected as representative samples of parallel experiments (selected The live pigs in this time period are used as test samples because the illegal addition of ractopamine in actual breeding is used in the time period before slaughter, and the selection of live pigs in this time period can make the pig urine matrix prepared by this method closer to actual status). After formulating feed containing a certain concentration of ractopamine, feed pigs regularly. At the same time, pig urine was continuously collected in a clean sample bottle, and the content of ractopamine was determined. Through the continuous and uninterrupted detection of pig urine samples obtained from 12 samples, it was found that the following general rules were foun...

Embodiment 2

[0032] Embodiment 2 homogeneity test

[0033] Randomly select 11 packaging units according to the whole packaging process before, during and after, and the randomly selected samples are numbered from 1 to 11, and each randomly selected unit takes 3 sub-samples in parallel, and the record numbers are 1-1, 1-2 , 1-3, 2-1, 2-2, 2-3, ..., 11-1, 11-2, 11-3. The homogeneity test method adopts liquid chromatography-isotope dilution mass spectrometry to measure the results (see the standard substance determination part for specific method parameters), and the results are statistically analyzed by analysis of variance, and judged by comparing the F test value with the F critical value. See Table 1 for the results of the homogeneity test and statistical analysis of the ractopamine components in pig urine.

[0034] Table 1 Pig urine matrix standard substance homogeneity test result containing ractopamine (ng / mL)

[0035]

[0036]

[0037] The above experimental data show that the...

Embodiment 3

[0038] Embodiment 3 Stability

[0039] Long-term stability monitoring studies were carried out at 0, 1, 3, 6, 9, and 12 months, respectively. Three packaging units are randomly selected each time, and each unit is measured in parallel three times. The measurement method is the same as that used in the homogeneity test, both of which are liquid chromatography-isotope dilution chromatography mass spectrometry. The average value of the measurement results of the three packaging units is taken as the long-term stability monitoring result. The trend analysis method is used to analyze the results, and the monitoring time and the results are fitted with a straight line, and the results are statistically analyzed. The long-term stability monitoring results of the pig urine lyophilized powder standard substance containing ractopamine are shown in Table 2. A straight line was fitted with the detection time and the results, and the trend analysis method was used to statistically analyze ...

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Abstract

The invention discloses a ractopamine standard substance coexisting in a conjugated state and a free state in a swine urine matrix as well as a preparation method and application of the ractopamine standard substance. The method includes: feeding animals with ractopamine to obtain a pig urine raw material, and valuing to obtain the free-state and conjugated-state coexisting ractopamine standard substance in the pig urine freeze-dried powder; adding water for redissolving into liquid, pre-treating the liquid by using a mixed biological enzyme enzymolysis method, and determining the content of ractopamine in the matrix standard substance by using a liquid chromatography-tandem mass spectrometry / isotope internal standard method for combined valuing. The standard substance prepared by the method provided by the invention can truly reflect the coexistence condition of the ractopamine standard substance in swine urine in a conjugated state and a free state after in-vivo metabolism of animals, and is more accurate in fixed value and good in uniformity and stability than a temporarily added and prepared standard substance in on-site rapid detection; therefore, the standard substance can be widely applied to the fields of ractopamine residue detection in animal urine, quality verification of rapid screening products, instrument detection method evaluation, laboratory internal quality control and the like.

Description

technical field [0001] The invention relates to the technical field of preparation of veterinary drug residue detection standard substances, in particular to a ractopamine standard substance co-existing in a conjugated state and a free state in pig urine freeze-dried powder after animal metabolism and a preparation method thereof. Background technique [0002] Ractopamine is beta 2 - One of the receptor agonists, it is also a poisonous and harmful compound that appeared earlier and is one of the most typical representatives of substances commonly known as "leptin". It is characterized by low cost and fast onset of action. It has been exposed to illegal and prohibited use in animal breeding many times, posing serious risks to human health and public health safety. Ractopamine has been included in the key monitoring parameters of animal food. At present, there are many methods for the determination of ractopamine residues in edible animal tissues such as pork and pig liver an...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/06G01N30/02G01N30/72
CPCG01N30/06G01N30/02G01N30/72
Inventor 单吉浩李建勋马康薛晓锋邢富国隋福顺卢培培赵玉乐徐迪
Owner INST OF AGRO FOOD SCI & TECH CHINESE ACADEMY OF AGRI SCI
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