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LC-MS method for the detection of various marine biotoxins in aquatic products

A technology for marine organisms and LC/MS, applied in measurement devices, instruments, scientific instruments, etc., can solve the problems of affecting the detection effect, the purification effect not meeting the requirements, and the loss.

Active Publication Date: 2021-09-21
NINGBO ACAD OF SCI & TECH FOR INSPECTION & QUARANTINE
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0009] For the complex matrix of aquatic products, the extract must be fully purified before instrumental analysis. The strong matrix effect of impurities such as fat can reduce the ionization efficiency of the target substance during the detection process of the liquid mass spectrometry instrument, seriously affecting the detection effect
If one of the above purification methods is selected alone, on the one hand, the purification effect may not meet the requirements; on the other hand, it will inevitably cause a large loss to one of the two types of targets with opposite physical and chemical properties, hydrophilic and lipophilic.

Method used

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  • LC-MS method for the detection of various marine biotoxins in aquatic products
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  • LC-MS method for the detection of various marine biotoxins in aquatic products

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0053] The detection objects are shown in Table 2, and the physical and chemical properties of the detected substances cover hydrophilicity and lipophilicity.

[0054] Table 2 List of standard substances

[0055]

[0056] (1) Materials and equipment

[0057] Main reagents and materials:

[0058] Unless otherwise specified, the listed reagents are chromatographically pure, and the water is the first-grade water specified in GB / T 6682.

[0059] Acetonitrile, methanol: HPLC grade; ammonia water, formic acid, ammonium formate, dimethyl sulfoxide: analytically pure. 0.1vol% formic acid: Take 1mL of formic acid and dilute to 1000mL with ultrapure water. Methanol-ammonia water (95+5): Add 5mL ammonia water to 95mL methanol. Mobile phase A: Aqueous solution containing 2mmol ammonium formate + 0.1vol% formic acid: Take 0.126g ammonium formate, 1mL formic acid, and dilute to 1000mL with ultrapure water; Mobile phase B: Acetonitrile-water solution of 2mmol ammonium formate + 0.1vo...

Embodiment 2

[0099] Embodiment 2 methodological verification

[0100] Select the blank matrix of yellow croaker and razor clam respectively, absorb an appropriate amount of mixed standard solution, so that the concentration of the target substance in the sample is 1, 2, and 5 times of the limit of quantification, operate according to the treatment process of the above method, and calculate the recovery rate and relative standard of sample addition after measurement. deviation.

[0101] Table 6 Standard recovery results

[0102]

[0103]

[0104] The results showed that the recoveries of all the above compounds ranged from 60.9% to 109.1%, and the precision ranged from 5.9% to 16.9%, which basically met the method verification requirements.

Embodiment 3

[0105] Embodiment 3 actual sample testing result:

[0106] Eight kinds of marine toxins were tested on the aquatic products yellow croaker and razor clam in the market, and the results are shown in Table 7

[0107] Table 7 sample test results

[0108]

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Abstract

The invention discloses a liquid mass spectrometry detection method for a variety of marine biological toxins in aquatic products. The samples of the aquatic products to be tested are extracted with 0.1vol% formic acid aqueous solution and acetonitrile in multiple stages, and the upper organic phase and the lower aqueous phase are obtained by layering. ; The lower aqueous phase was added to the MCX-HLB series column, rinsed with low-proportion methanol water, and then eluted once with the organic phase purified by dSPE, and then eluted with basic methanol for the second time. Liquid chromatography-tandem mass spectrometry is used for detection, and the external standard method is used for quantification to obtain the content of each component to be tested in the aquatic product sample to be tested. The invention can detect 8 kinds of marine biotoxins including hydrophilic and lipophilic at one time, and for the first time realizes one-step liquid mass spectrometry high-throughput quantitative detection of hydrophilic and lipophilic marine biotoxins.

Description

technical field [0001] The invention relates to a liquid-mass spectrometry detection method for various marine biotoxins in aquatic products Background technique [0002] With the progress of society and the development of industry, environmental problems are becoming more and more serious. Some industrial waste water and domestic sewage enter rivers, lakes and seas, resulting in eutrophication of water bodies and the proliferation of algae in water bodies. In particular, many marine red tide algae can produce toxins and accumulate in shellfish and other marine animals. Seafood contaminated by toxins can harm the digestive system, nervous system or cardiovascular system in the human body after being eaten by consumers, leading to human poisoning. even death. Common types of marine biotoxins in commercially available seafood include Paralytic Shellfish Poisoning (PSP), Diarrhetic Shellfish Poisoning (DSP), Amnesic Shellfish Poisoning (ASP), nervous Neurotoxic Shellfish Pois...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/02G01N30/06
CPCG01N30/02G01N30/06
Inventor 方科益陈树兵李双陈颖许迪明曹国洲
Owner NINGBO ACAD OF SCI & TECH FOR INSPECTION & QUARANTINE
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