Detection method for tiamulin and valnemulin in aquatic product

A tiamulin and detection method technology, applied in the detection field of tiamulin and vonemulin, can solve the problems of poor accuracy, low recovery rate and sensitivity, etc., to avoid rapid rise, improve grinding speed and effect, the effect of increasing friction

Pending Publication Date: 2020-01-21
MARINE FISHERIES RES INST OF ZHEJIANG
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] According to existing literature reports at present, the detection method of tiamulin and warnemulin mainly includes gas chromatography (GC), high performance liquid chromatography (HPLC) and high performance liquid chromatography-tandem mass spectrometry (HPLC-MS / MS) etc., and the above-mentioned method exists the low recovery rate and sensitivity, the defective of poor accuracy

Method used

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  • Detection method for tiamulin and valnemulin in aquatic product
  • Detection method for tiamulin and valnemulin in aquatic product
  • Detection method for tiamulin and valnemulin in aquatic product

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0049] (1) Sample pretreatment: place the fish meat of the above-mentioned crucian carp in a film bag and then slightly freeze it, then grind the slightly frozen sample intermittently to obtain a homogeneous sample, and grind intermittently for 2 seconds and stop for 1 second;

[0050] (2) Extraction: Add 10 mL of acetonitrile to 1.0 g homogeneous sample for ultrasonic extraction for 10 min, then centrifuge to get the supernatant; repeat the above operation with acetonitrile to extract the centrifuged solid once, combine the supernatants extracted twice, add acetonitrile volume to 25mL to obtain the extract;

[0051] (3) Purification: Take 10mL of the extract and place it in a centrifuge tube pre-added with 30g of N-propylethylenediamine (PSA), vortex for 2min, then centrifuge at 5000r / min for 5min, and take the supernatant;

[0052] (4) Concentration and transfer: take 5mL supernatant and dry it with nitrogen at 40°C, dissolve it with the mixture of mobile phase A and mobile ...

Embodiment 2

[0055] (1) Sample pretreatment: place the gills of the above-mentioned crucian carp in a film bag and seal them, then slightly freeze them, and grind the slightly frozen samples intermittently to obtain a homogeneous sample. The intermittent grinding is 2 seconds and stopped for 1 second;

[0056] (2) Extraction: Add 10 mL of acetonitrile to 1.0 g homogeneous sample for ultrasonic extraction for 10 min, then centrifuge to get the supernatant; repeat the above operation with acetonitrile to extract the centrifuged solid once, combine the supernatants extracted twice, add acetonitrile volume to 25mL to obtain the extract;

[0057] (3) Purification: take 10mL of the extract and place it in a centrifuge tube pre-added with 40g of N-propylethylenediamine (PSA), vortex for 3min, then centrifuge at 5500r / min for 6min, and take the supernatant;

[0058] (4) Concentration and transfer: take 5mL supernatant and dry it with nitrogen at 40°C, dissolve it with the mixture of mobile phase A...

Embodiment 3

[0061] (1) Sample pretreatment: place the heart of the above-mentioned crucian carp in a film bag and seal it, then micro-freeze it, grind the micro-frozen sample intermittently to obtain a homogeneous sample, and grind intermittently for 3 seconds, then stop for 1 second;

[0062] (2) Extraction: Add 12 mL of acetonitrile to 1.0 g homogeneous sample for ultrasonic extraction for 15 minutes, centrifuge to get the supernatant; repeat the above operation with acetonitrile to extract the centrifuged solid once, combine the supernatants extracted twice, add acetonitrile volume to 25mL to obtain the extract;

[0063] (3) Purification: Take 10mL of the extract and place it in a centrifuge tube pre-added with 50g of N-propylethylenediamine (PSA), vortex for 5min, then centrifuge at 6000r / min for 8min, and take the supernatant;

[0064] (4) Concentration and transfer: take 5mL supernatant and dry it with nitrogen at 40°C, dissolve it with the mixture of mobile phase A and mobile phase...

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Abstract

The invention discloses a detection method for tiamulin and valnemulin in an aquatic product. The detection method comprises the following steps of (1) sample pre-processing; (2) extraction; (3) purification; and (4) concentration and conversion solution. A dispersive solid-phase extraction-ultra high performance liquid chromatography-tandem mass spectrometry measurement technology is employed, the experiment efficiency is improved by optimizing instrument condition, sample pre-processing, extraction mode and PSA purification condition, the detection limit of the method is 0.1 microgram / kg, the recycling rate is 82.5-95.4%, the method is high in sensitivity, good in accuracy and reproducibility and high in applicability, the detection limit, the quantization limit and the recycling rate all can conform to the quality detection requirement of the aquatic product, and rapid detection of residue of veterinary drugs such as the tiamulin and the valnemulin is achieved.

Description

technical field [0001] The invention relates to the technical field of detection of tiamulin and warnemulin, in particular to a detection method for tiamulin and warnemulin in aquatic products. Background technique [0002] In the 1950s, scholars isolated pleuromutilin from the higher fungi Pleurotus multilus (Fr.) Sacc. and P. passecke-rianus Pilat, which is a diterpene compound with antibacterial activity. 5-6-8 three-membered ring backbone with neutral carbon atoms and a glycolate side chain. Tiamulin and warnemulin are chemically modified pleuromutilins with strong anti-drug-resistant bacteria activity. They were first developed for the prevention and treatment of Gram-positive bacteria, mycoplasma and other diseases. [0003] Tiamulin and warnemulin have the characteristics of broad antibacterial spectrum and low toxicity, and have good antibacterial properties against Mycoplasma genitalium, Treponema suis and aquatic products. Studies have shown that a small amount o...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/06G01N30/14G01N30/08G01N30/72
CPCG01N30/02G01N30/06G01N30/14G01N30/08G01N30/72G01N2030/062G01N2030/146
Inventor 曾军杰陈页卢义博
Owner MARINE FISHERIES RES INST OF ZHEJIANG
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