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Adopt sle method to separate the method for salbutamol in pig urine

A technology for salbutamol and pig urine, which is applied in the field of separating salbutamol in pig urine by SLE method, can solve the problems such as undetectable residual items, and achieve the effects of low detection limit, good separation efficiency and short separation time

Active Publication Date: 2016-11-23
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 application, in order to separate albuterol from protein, it is necessary to use enzymatic hydrolysis, and then through chromatographic detection after extraction by traditional methods, sometimes the residues cannot be detected

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  • Adopt sle method to separate the method for salbutamol in pig urine
  • Adopt sle method to separate the method for salbutamol in pig urine

Examples

Experimental program
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Effect test

Embodiment 1

[0019] Step 1: Collect 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 phosphate buffer solution with a pH of 6.5, centrifuge after mixing with a vortex mixer; take 0.5ml of supernatant after centrifugation; the mass ratio of trichloroacetic acid and pig urine is 1:99.

[0020] Step 2: After adding the supernatant to the SLE column, let it stand for 3 minutes; the SLE column is a medium liquid-liquid extraction SLE column produced by Orbi Shandong Technology Co., Ltd.

[0021] Step 3: Use the binary eluent to elute the SLE column twice, receive the eluent, and obtain the eluent containing salbutamol; the eluent consumed each time is 0.5ml, and the binary eluent is A mixture of ethyl acetate and acetonitrile, wherein the weight ratio of ethyl acetate to acetonitrile is 1:1.

Embodiment 2

[0023] Step 1. Collect 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 phosphate buffer solution with a pH of 7, centrifuge after mixing with a vortex mixer; take 0.5ml of the supernatant after centrifugation; the mass ratio of trichloroacetic acid and pig urine is 1:98.

[0024] Step 2: After adding the supernatant to the SLE column, let it stand for 4 minutes; the SLE column is a medium liquid-liquid extraction SLE column produced by Orbi Shandong Technology Co., Ltd.

[0025] Step 3: Use the binary eluent to elute the SLE column twice, receive the eluent, and obtain the eluent containing salbutamol; the eluent consumed each time is 0.5ml, and the binary eluent is A mixture of ethyl acetate and acetonitrile, wherein the weight ratio of ethyl acetate and acetonitrile is 1:1.1.

[0026] Standard s...

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Abstract

The invention discloses a method for separating salbutamol in pig urine by using the SLE method, which comprises the following steps: Step 1: sample pretreatment; collect pig urine, first add β-glucuronidase / arylsulfatase to enzymatically After enzymatic hydrolysis, add trichloroacetic acid to precipitate protein in pig urine, add phosphate buffer solution with 4 times the volume of pig urine with a pH range of 6.5 to 7.0, mix with a vortex mixer and centrifuge; take the supernatant after centrifugation; Step 2: After adding the supernatant to the SLE column, let it stand for 2 to 4 minutes; Step 3: Use the binary eluent to elute the SLE column at least twice, receive the eluate, and obtain the eluate containing albuterol . The object of the present invention is to provide a kind of method that adopts SLE method to separate albuterol in pig urine with high separation efficiency, simple operation and low detection limit.

Description

technical field [0001] The invention relates to the field of salbutamol detection, in particular to a method for separating salbutamol in pig urine by using the 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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IPC IPC(8): G01N30/14
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
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