Method for detecting beta-receptor agonist residual quantity in animal derived food

A receptor agonist, animal-derived technology, applied in the field of analytical chemistry, can solve the problems of lack of detection efficiency and cost, long processing time and high cost, and achieve improved detection time and cost, shortened detection time, and high accuracy. Effect

Active Publication Date: 2017-02-15
罗牛山腾德检测认证服务(海南)有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the enzymatic hydrolysis step of the detection method in this national standard requires the use of β-glucuronidase / arylsulfatase enzymatic hydrolysis. The cost of this enzyme is relatively high and the water bath hydrolysis treatment time is as long as 12 hours. In terms of detection efficiency and cost, this method It is lacking and is not suitable for the detection of large batches of samples

Method used

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  • Method for detecting beta-receptor agonist residual quantity in animal derived food
  • Method for detecting beta-receptor agonist residual quantity in animal derived food
  • Method for detecting beta-receptor agonist residual quantity in animal derived food

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0061] Embodiment 1: detection method of the present invention

[0062] Take the β-receptor agonist mixed standard working solution with a concentration of 1 μg / mL, dilute it into a 100 ng / mL mixed standard working solution, take 0 μL, 12.5 μL, 25 μL, 50 μL, 100 μL, and 250 μL respectively with 2% formic acid / water- The methanol solution was dissolved and the volume was adjusted to 0.5 mL. Then liquid chromatography tandem mass spectrometry detects, obtains standard curve;

[0063] Accurately weigh 5.00g of the sample to be tested in a 50ml centrifuge tube, add 100uL of 100ng / mL isotope internal standard working solution, then add 20.0mL of 0.1mol / L hydrochloric acid solution, add to a boiling water bath and boil for 30min, ultrasonically extract for 10min, use Adjust the pH to 9.5±0.1 with 10mol / L NaOH solution, centrifuge to take the supernatant, add 10mL of ethyl acetate to extract, vortex for 2min, centrifuge to take the organic phase and put it in another centrifuge tube...

Embodiment 2

[0067] Example 2: Linearity and working curve range

[0068] Prepare clenbuterol hydrochloride, ractopamine, and albuterol 2.5ng / mL, 5ng / mL, 10ng / mL, 20ng / mL, 50ng / mL gradient concentration standard working solutions for detection, and prepare working curves. The results are shown in Figure 1-3 , Table 4-5.

[0069] Table 4 The peak area of ​​clenbuterol hydrochloride, ractopamine and salbutamol concentration

[0070]

[0071] Table 5 Linear relationship between clenbuterol hydrochloride, ractopamine and albuterol

[0072] Substance name slope intercept Linear Fit Correlation Coefficient Clenbuterol Hydrochloride 1.523593 0.042159 0.9991 Ractopamine 1.364837 0.11713 0.9984 salbutamol 0.878222 0.003971 0.9989

[0073] From the above results, it can be known that the linear fitting correlation coefficients are all higher than 0.990, the curve meets the requirements, and the applicable concentration range is 0.25-5 μg / kg.

Embodiment 3

[0074] Embodiment 3: detection limit and quantitative limit

[0075] Prepare clenbuterol hydrochloride, ractopamine and salbutamol 2.5ng / mL respectively, repeat the measurement at least 6 times, collect the signal-to-noise ratio, statistical detection limit and quantification limit for each time, and the results are shown in Table 6.

[0076] Table 6 Limits of detection and limits of quantitation

[0077]

[0078] As can be seen from the above table, the detection limit of the present invention is far lower than the reported detection limit, which not only meets the requirements, but also has higher sensitivity.

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Abstract

The present invention relates to the technical field of analytical chemistry, and discloses a method for detecting beta-receptor agonist residual quantity in animal derived food, the method is based on a GB / T22286-2008 detection method, and aims at the defects of a long enzymolysis step for sample extraction of the GB / T22286-2008 detection method, a new sample processing step without enzymolysis is provided, detection time and cost are improved significantly, and the method has high accuracy, sensitivity and precision, and is suitable for detection of large quantities of samples.

Description

technical field [0001] The invention relates to the technical field of analytical chemistry, in particular to a method for detecting residues of beta-receptor agonists in animal-derived foods. Background technique [0002] β-receptor agonists are a class of chemically synthesized phenylethanolamines, the representative compounds are albuterol, terbutaline, cemanterol, cybuterol, ractopamine, clenbuterol (clenbuterol) , bromoclenbuterol, bromobuterol, phenoxypropofolamine, mabuterol, and mapenterol were mainly used to prevent and treat bronchial asthma and bronchospasm in humans and animals in the early days. Drugs like these have the effect of redistribution of nutrients and can significantly increase the lean meat percentage of animals, so they have been widely concerned as growth-promoting additives. However, people will experience adverse reactions such as flushing, headache, dizziness, chest tightness, heart palpitations, and numbness of limbs after eating livestock and...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02
CPCG01N30/02
Inventor 李雅岳君李达华崔梁伟
Owner 罗牛山腾德检测认证服务(海南)有限公司
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