Method for detecting tylosin residual titer in fungus residue

A technology of tylosin and detection method, which is applied in the field of detection of tylosin residual titer in bacterial residues, can solve the problems such as inability to detect tylosin residues quickly/accurately, and achieves reducing influence and improving accuracy. degree of effect

Inactive Publication Date: 2018-06-26
NINGXIA HOPE FIELD BIOLOGICAL AGRI TECH CO LTD
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

And to solve the problem that there is no effective solution to the influence of the matrix effect, and the existing technology cannot quickly / accurately detect the residual amount of tylosin in the bacteria residue,

Method used

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  • Method for detecting tylosin residual titer in fungus residue
  • Method for detecting tylosin residual titer in fungus residue
  • Method for detecting tylosin residual titer in fungus residue

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Experimental program
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specific Embodiment approach 1

[0037] Specific embodiment one: the detection method of the residual potency of tylosin in a kind of bacterial residue of the present embodiment, it is carried out according to the following steps:

[0038] 1. Sample preparation for the test product:

[0039] 1) Weigh the bacterial residue containing tylosin, add the extractant, vortex for 1-5min, then assisted extraction in ultrasound for 20-30min, centrifuge at 3000-4000rpm for 5-10min, take the supernatant, and collect the precipitate spare;

[0040] 2) Add the extractant to the precipitate collected in the previous step, vortex for 1 min, then assisted extraction in ultrasonic for 30 min, centrifuge at 3000-4000 rpm for 10 min, and take the supernatant;

[0041] 3) Combine the supernatants of step 1) and step 2), and rotate the supernatant in a 40°C water bath to 1 / 4 to 1 / 5 of the original volume to obtain an inorganic phase, and add methanol solution and pH to the inorganic phase Sodium acetate buffer solution with a co...

specific Embodiment approach 2

[0058] Embodiment 2: This embodiment differs from Embodiment 1 in that the eluent is an aqueous solution containing 2% ammonia by volume and 5% methanol by volume. Others are the same as in the first embodiment.

specific Embodiment approach 3

[0059] Specific embodiment three: the difference between this embodiment and specific embodiment one is: the mass spectrometry condition of the online solid-phase extraction-ultrahigh pressure liquid chromatography-triple quadrupole liquid phase mass spectrometer adopts the multi-stage reaction monitoring mode, and adopts positive ion The mode detects the precursor ion and fragments of tylosin. Others are the same as in the first embodiment.

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Abstract

The invention relates to a method for detecting tylosin residual titer in fungus residue. The method includes preparing a reference substance solution, preparing a test solution, adopting high-performance liquid chromatography-mass spectrometry to inject the reference substance solution and the test solution into a liquid chromatography-mass spectrometer in a gradient elution manner, and calculating the tylosin titer according to an external standard method. According to the method, a high-performance liquid chromatography-mass spectrometry detection and analysis method for the tylosin in thefungus residue is established through the optimization of the chromatographic conditions and tests of test sample and standard product preparation methods; through the optimization of a chromatogram and mass spectrometry system, a method for detecting the tylosin in fungus residue is established, and the method validation test researches show that the established method has high accuracy, strong specificity and good reproducibility, and can effectively detect the titer of tylosin in the fungus residue.

Description

technical field [0001] The invention relates to the technical field of detection and inspection of fungus residues, in particular to a method for detecting residual potency of tylosin in fungal residues. Background technique [0002] Biofermentation is one of the main production methods of antibiotics. Antibiotics can be synthesized through fermentation or drug intermediates and modified side chains. After extracting and purifying the target substance in the fermentation liquid, a large amount of bacterial residue is produced. my country is a big producer of antibiotics. These antibiotics will produce a large amount of antibiotic residue every year. According to 1 ton of antibiotics, 40 tons of wet bacterial residue will be produced (the moisture content is about 70%) According to calculations, in 2009, the wet fungus residue produced in one year reached about 6 million tons. Since the fungus residue is mainly inactivated mycelia, residual culture medium, microbial metabolit...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/06
CPCG01N30/02G01N30/06
Inventor 王义张鹏金昌福李宁飞
Owner NINGXIA HOPE FIELD BIOLOGICAL AGRI TECH CO LTD
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