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High-resolution mass spectrum detection method for lipophilic toxins in shellfish

A high-resolution mass spectrometry and detection method technology, applied in the field of high-resolution mass spectrometry detection of lipophilic toxins in shellfish, to achieve the effects of improving detection efficiency, shortening detection and processing time, and simplifying the pretreatment process

Inactive Publication Date: 2020-06-12
GUANGXI ACADEMY OF FISHERY SCI
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, there are very few methods in the prior art that can detect multiple lipophilic marine biotoxins at one time. Therefore, it is necessary to establish a method that can complete lipophilic marine biotoxins in shellfish at one time through reasonable selection of chromatographic columns and optimization of mass spectrometry parameters such as flow. Liquid-mass spectrometry method for high-throughput detection of biotoxins

Method used

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  • High-resolution mass spectrum detection method for lipophilic toxins in shellfish
  • High-resolution mass spectrum detection method for lipophilic toxins in shellfish
  • High-resolution mass spectrum detection method for lipophilic toxins in shellfish

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Embodiment 1

[0038] 1. Sample processing and testing:

[0039] Accurately weigh 5.00g (±0.01g) sample into a 50mL centrifuge tube, add 10mL methanol, vortex mix for 1min, ultrasonically extract for 5min, centrifuge at 8000rpm for 10min, transfer the supernatant to another centrifuge tube; Repeat the extraction once with 10 mL of methanol, and dilute the combined supernatant to 20 mL with methanol; add 1 g of anhydrous magnesium sulfate and 0.15 g of C18, shake vigorously for 1 min, and centrifuge at 8000 rpm for 5 min; Liquid chromatography-quadrupole-electrostatic orbitrap high-resolution mass spectrometry was used for determination.

[0040] Wherein, the liquid chromatography conditions in the qualitative and quantitative detection are as follows:

[0041] Chromatographic column: C18, the specification is 1.9μm, 2.1mm×100mm;

[0042] Mobile phase: A-acetonitrile; B-0.002mol / L ammonium formate solution, containing 0.2% formic acid;

[0043] Column temperature: 40°C;

[0044] Injection...

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Abstract

The invention belongs to the technical field of mass spectrometric detection, and discloses a high-resolution mass spectrometric detection method for lipophilic toxins in shellfish. The method comprises sample treatment and qualitative and quantitative detection, and the sample treatment method comprises the following steps: weighing a sample, putting the sample into a centrifuge tube, adding methanol, carrying out vortex uniform mixing, carrying out ultrasonic extraction, carrying out centrifuging, taking the supernatant, and transferring the supernatant into another centrifuge tube; repeatedly extracting residues once by using methanol, merging the supernatant, fixing the volume by using methanol, adding anhydrous magnesium sulfate and C18, violently performing oscillating, then carryingout centrifuging, and filtering the supernatant by using a filter membrane. The qualitative and quantitative detection comprises the step of performing determination by using a liquid chromatography-quadrupole rod-electrostatic orbitrap high-resolution mass spectrum after the sample is treated. The method can be used for qualitatively and quantitatively analyzing various lipophilic shellfish toxins at the same time, and has important reference significance for knowing the pollution condition of the shellfish toxins.

Description

technical field [0001] The invention relates to the technical field of mass spectrometry detection, in particular to a high-resolution mass spectrometry detection method for lipophilic toxins in shellfish. Background technique [0002] In recent years, shellfish farming has developed rapidly, and it is the dominant species mainly cultured along the coast of my country. Industrial wastewater and domestic sewage enter rivers, lakes and seas, leading to eutrophication of the water body, causing algae to multiply in the water body. Many marine red tide algae can produce toxins, and shellfish are filter-feeding animals that feed on phytoplankton and organic debris. Toxin-producing algae enter the food chain through the accumulation of shellfish, and after being eaten by consumers, they can harm the digestive system, nervous system, and cardiovascular system in the human body, leading to human poisoning and even death, bringing great food safety risks to consumers . [0003] Amo...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/06G01N30/14G01N30/72G01N30/54
CPCG01N30/02G01N30/06G01N30/14G01N30/72G01N30/54G01N2030/027G01N2030/062G01N2030/146
Inventor 吴祥庆杨姝丽谢宗升秦振发蒙源吴明媛
Owner GUANGXI ACADEMY OF FISHERY SCI
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