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Method for separating ractopamine in pig urine by sle method

A technology of ractopamine and pig urine, which is applied in the field of separating ractopamine in pig urine by SLE method, can solve the problem of undetectable residual items, and achieve the effect of short separation time and high separation efficiency

Active Publication Date: 2016-11-23
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

[0022] 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 ammonia-ammonium chloride buffer solution with a pH 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.

[0023] Step 2: After adding the supernatant to the SLE column, let stand for 3 minutes;

[0024] 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 dioxane, and the weight ratio of isopropanol and dioxane is 1:1.

Embodiment 2

[0026] 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 ammonia-ammonium chloride buffer solution with a pH of 9, 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.

[0027] Step 2: After adding the supernatant to the SLE column, let stand for 3 minutes;

[0028] 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 dioxane, and the weight ratio of isopropanol and dioxane is 0.8:1.

[0029] Standard sample preparation

[0030] Take by weighing 0.0100g of ractopamine standard substance (purity...

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Abstract

The invention discloses a method for separating ractopamine in pig urine by using the SLE method, comprising the following steps: Step 1: sample pretreatment; collecting pig urine, first adding β-glucuronidase / arylsulfatase hydrochloride to carry out For enzymatic hydrolysis, add β-glucuronidase / arylsulfatase 12 μL per ml of urine; take the supernatant after centrifugation; Step 2: Add the supernatant to the SLE column and let it stand for 2~ 4 minutes; step 3: use a binary eluent to elute the SLE column at least twice, receive the eluent, and obtain an eluent containing ractopamine; wherein, the binary eluent is isopropanol and di A mixture of oxane, wherein the weight ratio of isopropanol to dioxane is 0.5-1:1. The object of the present invention is to provide a method for separating ractopamine in pig urine by using the SLE method with high separation efficiency and simple operation.

Description

technical field [0001] The invention relates to the field of ractopamine detection, in particular to a method for separating ractopamine in pig urine by using an SLE method. 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 type...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/06
Inventor 陈学松赖秀梅温志芳陈启钊郭振旺吴岚
Owner WUZHOU INST FOR FOOD & DRUG CONTROL