Looking for breakthrough ideas for innovation challenges? Try Patsnap Eureka!

Method for determining content of tiamulin and valnemulin in veterinary drug preparation through solid phase extraction-high performance liquid chromatography-tandem mass spectrometry

A high-performance liquid chromatography, tiamulin technology, applied in the field of drug testing, can solve problems such as infection, antibiotic residue hazards, flora imbalance, etc., and achieve the effects of improving work efficiency, good linear relationship, and simple method

Pending Publication Date: 2022-07-15
石家庄海关技术中心
View PDF2 Cites 0 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

After a large amount of antibiotics enter the animal body, they quickly reach the main organs along with the blood circulation, breaking the normal flora balance in the animal body, causing flora imbalance, decreased immunity, and then causing various endogenous and exogenous bacterial infections. Thus endangering animal health, affecting the food safety of animal-derived food and the development of animal husbandry
[0005] 2. The harm of antibiotic residues to human body
3) Produce drug-resistant pathogenic bacteria; long-term intake of sub-dose antibiotics often leads to the emergence of drug-resistant strains in humans
In the prior art, there are only detection methods for salnimulin and tiamulin residues in feed, food and live fish for export, while the lack of detection methods in veterinary drug preparations has caused a blind spot in drug safety monitoring

Method used

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Image

Smart Image Click on the blue labels to locate them in the text.
Viewing Examples
Smart Image
  • Method for determining content of tiamulin and valnemulin in veterinary drug preparation through solid phase extraction-high performance liquid chromatography-tandem mass spectrometry
  • Method for determining content of tiamulin and valnemulin in veterinary drug preparation through solid phase extraction-high performance liquid chromatography-tandem mass spectrometry
  • Method for determining content of tiamulin and valnemulin in veterinary drug preparation through solid phase extraction-high performance liquid chromatography-tandem mass spectrometry

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0075] To prepare standard working solution:

[0076] Precisely weigh 10 mg of tiamulin and vornimulin respectively (accurate to 0.01 mg), dissolve in acetonitrile and dilute to 100 mL, and prepare a standard stock solution with a mass concentration of 100 mg / L; accurately pipette 1 mL of each The above stock solution was placed in a 100mL volumetric flask, and the mixed standard intermediate solution of 1.0 mg / L was prepared with acetonitrile; L, 5μg / L, 10μg / L, 20μg / L, 50μg / L, 100μg / L standard working solutions.

[0077] Sample pretreatment:

[0078] Weigh 1.0 g of sample (accurate to 0.01 g) into a 50 mL centrifuge tube with a stopper, add 20 mL of acetonitrile, cover and mix well, vortex on a vortex shaker for 5 min, and centrifuge at 4000 r / min for 5 min after extraction.

[0079] A MCX solid phase extraction cartridge (60 mg, 3 mL) was activated with 3 mL of methanol and equilibrated with 3 mL of 0.1% aqueous formic acid. Take 2mL of the above-mentioned acetonitrile ex...

experiment example 1

[0088] Chromatographic separation and mass spectrometry detection of the mixed solution of the analyte:

[0089] Method Linearity, Limits of Detection, and Limits of Quantitation

[0090] Under the experimental conditions determined by this method, the preparation concentrations were 1.0ng / mL, 2.0ng / mL, 5.0ng / mL, 10.0ng / mL, 20.0ng / mL, 30.0ng / mL, 50.0ng / mL, 100.0 Eight standard series of ng / mL were measured by LC / MS, and the response peak area (Y-axis) of quantitative ions was plotted against the corresponding mass concentration (X-axis, ng / mL). The results are shown in Table 3. The results showed that in the range of 1.0-100 ng / mL for tiamulin and vonimulin, there was a good linear relationship between the response peak area of ​​the quantitative ion and the sample concentration, and the correlation coefficients were all greater than 0.99. See image 3 and Figure 4 .

[0091] According to the sample amount represented by the final sample solution, the volume of constant vo...

experiment example 2

[0096] Matrix effect detection

[0097] Matrix effects (ME) refer to the ionization effect of co-eluted substances during chromatographic separation, resulting in the inhibition or enhancement of the signal. When the influence of matrix effect is large, it will reduce the sensitivity of the method and affect the accuracy of the method, which will bring errors to the determination. Therefore, it is necessary to evaluate the matrix effects (ME) in the process of liquid chromatography-mass spectrometry method development and confirmation. Matrix effect (%) ME = (slope of matrix-matched standard curve / slope of pure solvent standard curve) x 100%. It is generally believed that the matrix effect is not obvious when the matrix effect is between 85% and 115%. In this method, the standard working curve and matrix matching calibration curve are prepared, the peak area is taken as the ordinate and the mass concentration is plotted as the abscissa. figure 2 It shows that for the three ...

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

PUM

No PUM Login to View More

Abstract

The invention provides a method for determining the content of tiamulin and valnemulin in a veterinary drug preparation through solid phase extraction-high performance liquid chromatography-tandem mass spectrometry, and belongs to the technical field of drug detection. The invention provides a method for rapidly detecting tiamulin and valnemulin in a veterinary drug preparation through solid phase extraction / high performance liquid chromatography-tandem mass spectrometry. The method comprises the following steps: extracting a sample by using acetonitrile, purifying by using an MCX solid-phase extraction column, carrying out gradient elution on a C18 chromatographic column by using acetonitrile and a 0.1% formic acid aqueous solution as a mobile phase, and carrying out quantitative analysis in a liquid chromatography-tandem mass spectrometry MRM mode. The linear relation of the two detected compounds in the range of 1.0-100 ng / mL is good, the correlation coefficient is larger than 0.999, the detection limit of the method is 0.05 mg / kg, and the quantitation limit is 0.1 mg / kg. The method provided by the invention is simple, rapid and accurate, and can realize rapid determination of the veterinary drug preparation.

Description

technical field [0001] The invention relates to the technical field of drug detection, in particular to a method for determining the content of tiamulin and vonimulin in veterinary drug preparations by solid phase extraction-high performance liquid chromatography-tandem mass spectrometry. Background technique [0002] Valnemulin and Tiamulin both belong to pleuromutilin derivative antibiotics. Valnemulin and tiamulin belong to the same class of drugs and are a new generation of pleuromutilin semi-synthetic antibiotics. Antibiotics, in practical application, are usually used in the hydrochloride of vonimulin and the fumarate of tiamulin. Both Vonimulin and Tiamulin have broad-spectrum antibacterial properties. These antibiotics have antibacterial effects on Gram-positive bacteria and mycoplasma by inhibiting the synthesis of bacterial proteins, and can effectively kill various bacteria, streptococci and mycoplasma. , has the characteristics of strong antibacterial activity, ...

Claims

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

Application Information

Patent Timeline
no application Login to View More
IPC IPC(8): G01N30/02G01N30/06G01N30/72
CPCG01N30/02G01N30/06G01N30/72
Inventor 于趁田浩王敬窦彩云艾连峰
Owner 石家庄海关技术中心
Who we serve
  • R&D Engineer
  • R&D Manager
  • IP Professional
Why Patsnap Eureka
  • Industry Leading Data Capabilities
  • Powerful AI technology
  • Patent DNA Extraction
Social media
Patsnap Eureka Blog
Learn More
PatSnap group products

Browse by: Latest US Patents, China's latest patents, Technical Efficacy Thesaurus, Application Domain, Technology Topic, Popular Technical Reports.

© 2024 PatSnap. All rights reserved.Legal|Privacy policy|Modern Slavery Act Transparency Statement|Sitemap|About US| Contact US: help@patsnap.com