Method for high-precisely measuring salbutamol in swine urine

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

Active Publication Date: 2015-09-23
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

[0029] 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 Phosphate buffer 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.

[0030] 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.

[0031] 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 cyclohexane, wherein the weight ratio of ethyl acetate and cyclohexane is 1:1.

Embodiment 2

[0033] 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.

[0034] 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.

[0035] 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 cyclohexane, wherein the weight ratio of ethyl acetate and cyclohexane is 1:1.2.

[0036] Standard sam...

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Abstract

The invention discloses a method for high-precisely measuring salbutamol in swine urine. The method comprises the following steps: step 1: pretreating a sample; collecting swine urine, firstly carrying out enzymolysis by charging beta-hydrochloric glucuronidase / aryl sulfatase, charging trichloroacetic acid to precipitate proteins in the swine urine, charging a phosphoric acid buffer solution with volume being 4 times of that of the swine urine and with pH value of 6.5 to 7.0, mixing by a vortex mixer, and then centrifuging; taking the supernatant of the centrifuged solution; step 2: charging the supernatant into an SLE column, and standing for 2 to 4 minutes; step 3: eluting the SLE column for at least two times by adopting a binary elution agent, collecting the elution solution, and obtaining the elution solution containing salbutamol; step 4: detecting the elution solution obtained in the step 3 by adopting a high-efficiency liquid-phase chromatography. The invention aims at providing the method for measuring the content of salbutamol in the swine urine, which is high in separation efficiency, simple to operate and high in precision.

Description

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

Claims

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Application Information

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IPC IPC(8): G01N30/02
Inventor 陈学松吴岚邓水德赖秀梅蔡姬灵
Owner WUZHOU INST FOR FOOD & DRUG CONTROL
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