Method for high-precision measurement of ractopamine, clenbuterol, and albuterol in pig urine

A technology of ractopamine and salbutamol, which is applied in the field of detection of animal tissues and excrement, can solve the problem of inability to detect residual items, and achieve the effects of reducing the difficulty of detection, improving the separation efficiency and improving the detection accuracy.

Active Publication Date: 2016-07-06
WUZHOU INST FOR FOOD & DRUG CONTROL
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] Announcement No. 1025 of the Ministry of Agriculture-11-2008 discloses the detection of multiple residues of β-receptor agonists in pig urine, which is extracted with isopropanol-ethyl acetate after enzymatic hydrolysis, and the relevant detection results can be obtained by internal standard method , but in practical applications, residues cannot be detected by chromatographic detection after enzymatic hydrolysis and extraction by traditional methods

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] Step 1: Take 1 g of pig urine, first add 12 μL β-glucuronidase hydrochloride / arylsulfatase for enzymatic hydrolysis, the enzymatic hydrolysis time is 3-4 hours, after the enzymatic hydrolysis, add trichloroacetic acid to precipitate the protein in pig urine , adding 4ml of Ph is the ammonium acetate buffer solution of 5.6, and centrifuges after mixing with a vortex mixer; get 0.5ml of supernatant after centrifugation; the mass ratio of trichloroacetic acid and pig urine is 1:99.

[0029] Step 2: After adding the supernatant to the SLE column, let stand for 3 minutes;

[0030] Step 3: Use the binary eluent to elute the SLE column twice, receive the eluent, and obtain the eluent containing ractopamine, clenbuterol, and salbutamol; the eluent consumed each time is 0.5ml, so The binary eluent described above is a mixture of n-butanol and methyl acetate, and the weight ratio of n-butanol and methyl acetate is 4:1.

Embodiment 2

[0032] Step 1: Take 1 g of pig urine, first add 12 μL β-glucuronidase hydrochloride / arylsulfatase for enzymatic hydrolysis, the enzymatic hydrolysis time is 3-4 hours, after the enzymatic hydrolysis, add trichloroacetic acid to precipitate the protein in pig urine , add 4ml of Ph is the ammonium acetate buffer of 5.8, centrifuge after mixing with a vortex mixer; take 0.5ml of supernatant after centrifugation; the mass ratio of trichloroacetic acid and pig urine is 1:100.

[0033] Step 2: After adding the supernatant to the SLE column, let stand for 3 minutes;

[0034] Step 3: Use the binary eluent to elute the SLE column twice, receive the eluent, and obtain the eluent containing ractopamine, clenbuterol, and salbutamol; the eluent consumed each time is 0.5ml, so The binary eluent described above is a mixture of n-butanol and methyl acetate, and the weight ratio of n-butanol and methyl acetate is 5:1.

[0035] Standard sample preparation

[0036] Take by weighing ractopamine...

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Abstract

The invention discloses a method for measuring the content of ractopamine, clenbuterol and albuterol in pig urine with high precision, comprising the following steps: Step 1: sample pretreatment; collecting pig urine, first adding β-glucuronidase hydrochloride / arylsulfatase for enzymatic hydrolysis; take the supernatant after centrifugation; step 2: add the supernatant to the SLE column and let it stand for 2 to 4 minutes; step 3: use binary eluent to clean the SLE column Elute at least twice, receive the eluate, and obtain the eluate containing ractopamine, clenbuterol, and salbutamol. Step 4: Use high performance liquid chromatography to detect the eluate obtained in step 3. The object of the present invention is to provide a method for measuring the contents of ractopamine, clenbuterol and albuterol in pig urine with high precision.

Description

technical field [0001] The invention relates to the detection field of animal tissue and excrement, in particular to a method for measuring the contents of ractopamine, clenbuterol and salbutamol in pig urine with high precision. Background technique [0002] Sample pretreatment is a key link in the analysis and detection process. It is an important means to concentrate the trace components to be determined, improve the sensitivity of the method, and remove substances that interfere with the analysis system. Extraction is a technique to separate the target compound from the sample mass, and it is one of the most important methods in sample pretreatment. At present, liquid-liquid extraction is still one of the most widely used sample preparation methods. However, the traditional liquid-liquid extraction is cumbersome and time-consuming, consumes a lot of organic solvents, and is prone to emulsification, which makes it have certain advantages in practical applications. limita...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/88
Inventor 陈学松郭振旺黄蘅吴岚邓水德黎志锐
Owner WUZHOU INST FOR FOOD & DRUG CONTROL
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