Method for detecting menbutone residues in porcine tissues

A technology of menbutone and tissue, applied in the field of analysis, can solve the problems of many side effects, small safety range, poor selectivity, etc., and achieve the effect of simple operation, high sensitivity and good accuracy

Active Publication Date: 2015-12-30
SOUTHWEST UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

In the clinical treatment of such diseases or symptoms, bethanechol, neostigmine methosulfate, concentrated sodium chloride injection and other cholinomimetic or anticholinesterase drugs are often used. Poor sex, many side effects, high toxicity, small safety range

Method used

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  • Method for detecting menbutone residues in porcine tissues
  • Method for detecting menbutone residues in porcine tissues
  • Method for detecting menbutone residues in porcine tissues

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] Embodiment 1, the establishment of the residual detection method of monbutronone in porcine tissue

[0032] The method for detecting residues of menbutronone in porcine tissue, the specific steps are as follows:

[0033] (1) Pretreatment of tissue samples: Weigh 20 g of porcine tissue (muscle, fat, liver or kidney) after intramuscular injection of menbutrin injection, chop it up, and place it in a high-speed disperser (endo-type homogenizer), Homogenize at 6000r / min for 8min, then accurately weigh 2.0g of the homogenized tissue, add 4mL of acetonitrile, vortex mix, centrifuge at 3000r / min for 10min, take the supernatant, add acetonitrile repeatedly to extract 2 Combine the supernatants extracted three times, then transfer all the supernatants to a 50mL round-bottomed flask, and evaporate to dryness in vacuum at 60°C. The phase was ultrasonically dissolved and transferred to a centrifuge tube, and centrifuged at 10,000r / min for 10min, and the centrifuged supernatant was...

Embodiment 2

[0036] Embodiment 2, verification of tissue sample pretreatment method

[0037] (1) Homogenization speed

[0038] Take respectively 5 parts of pig's muscle (non-injection site and injection site), fat, liver and kidney after intramuscular injection of menbutronone injection, each part of about 20.0g, respectively at 2800, 4000, 5000, 6000, 7000r / Homogenize for 8 minutes under the condition of 1 min, and then operate according to the method of Example 1. Each tissue takes 2 parts of the test sample, and each part is continuously injected 2 times for analysis, and the reference substance solution is continuously injected 5 times. Calculated according to the external standard method. The average monbutronone content at the homogenization rotation speed, and calculate the relative deviation of the average monbutronone content between adjacent rotation speeds, the results are shown in Tables 1-5.

[0039] Table 1. Effects of different homogenization speeds on the determination of...

Embodiment 3

[0091] Embodiment 3, verification of the residual detection of menbutronone

[0092] The verification was carried out in accordance with the requirements of the Ministry of Agriculture document "Technical Specifications for Veterinary Drug Residue Testing (Trial)".

[0093] The specific chromatographic conditions are as follows: the chromatographic column is Shim-packVP-ODSC 18 Column (4.6×250mm, 5μm), octadecylsilane bonded silica gel as filler; mobile phase is acetonitrile and 0.5% phosphoric acid (55:45 by volume); column temperature is 25°C; detection wavelength is 235nm; flow rate The injection volume is 20 μL; the number of theoretical plates is not less than 2000 based on the monbutronone peak, and the separation degree between the monbutronone peak and the adjacent impurity peak is greater than 1.5.

[0094] Verification method: Accurately weigh 10 mg of menbutrin reference substance, dissolve it in acetonitrile and dilute to 100 mL, shake well, accurately measure 5.0...

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Abstract

The invention discloses a method for detecting a menbutone residue in pig tissue. The method comprises the steps as follows: firstly, the pig tissue subjected to intramuscular menbutone injection is weighed, cut up and then subjected to homogenate, and the tissue subjected to homogenate is extracted by using acetonitrile, then after centrifugation, the extracted liquid is subjected to rotary evaporation in vacuum with the temperature of 60 DEG C to dry, and after cooling, moving phase is added into the residue for ultraphonic dissolution and then centrifugation, and a liquid supernatant is collected and filtered by a millipore filter membrane with filtering particle diameter of 0.22 mu m, and the filter liquor is used as a test solution; secondly, a menbutone reference substance is weighed precisely, and after dissolved by acetonitrile and diluted by moving phase, the reference substance has a concentration of 9 to 11 mu g / mL, and a reference substance solution is obtained; thirdly, HPLC (High-Performance Liquid Chromatography) is adopted for testing the test solution and the reference substance solution, the chromatogram is recorded, and the menbutone residue in the tissue is calculated by peak area according to external standard method. The method is good in specificity, high in sensitivity and good in repeatability, can quickly detect the menbutone residue in the pig tissue, and is a reliable method for controlling the quantity of the menbutone residue in animal-origin food.

Description

technical field [0001] The invention belongs to the technical field of analysis, and in particular relates to a method for detecting monbuterone residues in porcine tissues. Background technique [0002] Digestive system diseases often occur during the growth of animals. Gastrointestinal dysfunction such as indigestion, loss of appetite, constipation and abdominal distension often hinder the growth and development of animals and hinder the development of the breeding industry. In the clinical treatment of such diseases or symptoms, bethanechol, neostigmine methosulfate, concentrated sodium chloride injection and other cholinomimetic or anticholinesterase drugs are often used. Poor sex, many side effects, high toxicity, and small safety range. [0003] Menbutone is a special choleretic agent for animals, which can promote the secretion of bile, gastric juice and pancreatic juice, thereby increasing the supply of cholate, pepsin, trypsin, pancreatic amylase, pancreatic lipase...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/02G01N30/06
Inventor 罗雷钟红罗永煌胡昌华伍莉杨游谭明国王小红龚晶雯吴梦婉王帅龙飞
Owner SOUTHWEST UNIV
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