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High-accuracy measuring method for clenbuterol content in swine urine

A high-precision, pig urine technology, used in measuring devices, instruments, scientific instruments, etc., can solve problems such as inability to detect residual items, and achieve the effects of improved measurement accuracy, short separation time, and good separation efficiency.

Inactive Publication Date: 2015-07-29
WUZHOU INST FOR FOOD & DRUG CONTROL
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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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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  • High-accuracy measuring method for clenbuterol content in swine urine

Examples

Experimental program
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Effect test

Embodiment 1

[0028] Step 1: Collect 1ml of pig urine, add trichloroacetic acid to precipitate protein in pig urine, add 4ml of 2mol / L ammonium acetate buffer solution, mix with a vortex mixer and centrifuge; take 0.5ml of the centrifuged supernatant; The mass ratio of chloroacetic acid to pig urine is 1:99; the specific operation of the centrifugal treatment is: centrifuging the mixed solution in a centrifuge at a speed of 10000 rpm for 0.8 minutes.

[0029] Step 2: After adding the supernatant to the SLE column (medium liquid-liquid extraction SLE column produced by Orbi Shandong Science and Technology Co., Ltd.), 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 clenbuterol; the eluent consumed each time is 0.5ml, and the binary eluent The removing agent is a mixture of ethyl acetate and methyl acetate, and the weight ratio of ethyl acetate and methyl acetate is 1:0.8.

Embodiment 2

[0032] Step 1: Collect 1ml of pig urine, add trichloroacetic acid to precipitate protein in pig urine, add 4ml of 2mol / L ammonium acetate buffer solution, mix with a vortex mixer and centrifuge; take 0.5ml of the centrifuged supernatant; The mass ratio of chloroacetic acid to pig urine is 1:98; the specific operation of the centrifugation process is: centrifuge the mixed solution in a centrifuge at a speed of 9000 rpm for 1 minute.

[0033] Step 2: After adding the supernatant to the SLE column (medium liquid-liquid extraction SLE column produced by Orbi Shandong Science and Technology Co., Ltd.), let stand for 2 minutes;

[0034] Step 3: Use the binary eluent to elute the SLE column twice, receive the eluent, and obtain the eluent containing clenbuterol; the eluent consumed each time is 0.5ml, and the binary eluent The removing agent is a mixture of ethyl acetate and methyl acetate, and the weight ratio of ethyl acetate and methyl acetate is 1:1.

Embodiment 3

[0036] Step 1: Collect 1ml of pig urine, add trichloroacetic acid to precipitate protein in pig urine, add 4ml of 2mol / L ammonium acetate buffer solution, mix with a vortex mixer and centrifuge; take 0.5ml of the centrifuged supernatant; The mass ratio of chloroacetic acid to pig urine is 1:99; the specific operation of the centrifugation treatment is: centrifuge the mixed solution in a centrifuge at a speed of 10000 rpm for 0.5 minutes.

[0037] Step 2: After adding the supernatant to the SLE column (medium liquid-liquid extraction SLE column produced by Orbi Shandong Science and Technology Co., Ltd.), let stand for 4 minutes;

[0038] Step 3: Use the binary eluent to elute the SLE column twice, receive the eluent, and obtain the eluent containing clenbuterol; the eluent consumed each time is 0.5ml, and the binary eluent The removing agent is a mixture of ethyl acetate and methyl acetate, and the weight ratio of ethyl acetate and methyl acetate is 1:0.5.

[0039] Standard sa...

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Abstract

The invention discloses a high-accuracy measuring method for the clenbuterol content in swine urine. The high-accuracy measuring method comprises the following steps of the step 1 of preprocessing samples, collecting swine urine, adding trichloroacetic acid to precipitate protein in the swine urine, adding 80%VOL 2mol / L ammonium acetate buffer solution, centrifuging the solution through a whirlpool mixer after being mixed and taking centrifuged liquid supernatant; the step 2 of adding the liquid supernatant into an SLE column and standing for 2 to 4 minutes; the step 3 of eluting the SLE column through binary eluent at least twice, receiving the eluent and obtaining the eluent containing clenbuterol; the step 4 of detecting the eluent obtained in the step 3 through a high-efficiency liquid chromatography. The high-accuracy measuring method for the clenbuterol content in the swine urine is good in separating effect and facilitates follow-up testing work.

Description

technical field [0001] The invention relates to the detection field of animal feed, in particular to a method for measuring clenbuterol content 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. limitations. [0003] In 1998, scientists proposed a new ...

Claims

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Application Information

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IPC IPC(8): G01N30/02
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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