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Method for measuring content of ractopamine in swine urine at high precision

A ractopamine and high-precision technology, which is applied in the detection field of animal feed, can solve the problems of undetectable residual items, etc., and achieve the effects of improved measurement accuracy, good separation efficiency, and short separation time

Active Publication Date: 2015-07-29
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

[0029] Step 1: Take 1ml of pig urine, first add 12μL β-glucuronidase hydrochloride / arylsulfatase for enzymolysis, the enzymolysis time is 3-4 hours, after the enzymolysis, add trichloroacetic acid to precipitate the protein in pig urine , add 4ml of Ph to the ammonia-ammonium chloride buffer solution of 9, centrifuge 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.

[0030] Step 2: After adding the supernatant to the SLE column, let stand for 3 minutes;

[0031] Step 3: Elute the SLE column twice with a binary eluent, receive the eluent, and obtain an eluent containing ractopamine; the eluent consumed each time is 0.5ml, and the binary eluent It is a mixture of isopropanol and methyl acetate, and the weight ratio of isopropanol and methyl acetate is 1:1.

Embodiment 2

[0033] Step 1: Take 1ml of pig urine, first add 12μL β-glucuronidase hydrochloride / arylsulfatase for enzymolysis, the enzymolysis time is 3-4 hours, after the enzymolysis, add trichloroacetic acid to precipitate the protein in pig urine , add 4ml of Ph to the ammonia-ammonium chloride buffer solution of 9, centrifuge after mixing with a vortex mixer; get 0.5ml of supernatant after centrifugation; the mass ratio of trichloroacetic acid and pig urine is 1:100.

[0034] Step 2: After adding the supernatant to the SLE column, let stand for 3 minutes;

[0035] Step 3: Elute the SLE column twice with a binary eluent, receive the eluent, and obtain an eluent containing ractopamine; the eluent consumed each time is 0.5ml, and the binary eluent It is a mixture of isopropanol and methyl acetate, and the weight ratio of isopropanol and methyl acetate is 0.8:1.

[0036] Standard sample preparation

[0037] Weigh 0.0100 g of ractopamine standard substance (purity ≥ 99%), place in a 1000 ...

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Abstract

The invention discloses a method for measuring the content of ractopamine in swine urine at high precision. The method comprises the following steps: 1, pretreating a sample and collecting the swine urine; 2, adding supernate to an SLE (Supported Liquid Extraction) column and standing for 2 to 4 minutes; 3, eluting the SLE column for at least two times by adopting a binary eluent, and collecting an elution solution to obtain a ractopamine-containing elution solution; 4, detecting the elution solution obtained in the step 3 by adopting high performance liquid chromatography, wherein the binary eluent is a mixture of isopropanol and methyl acetate according to a weight ratio of (0.5 to 1): 1. The invention aims at providing the method for measuring the content of the ractopamine in the swine urine at high precision, which is high in separation efficiency and simple to operate.

Description

technical field [0001] The invention relates to the detection field of animal feed, in particular to a method for measuring the content of ractopamine 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...

Claims

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Application Information

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Patent Type & Authority Applications(China)
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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