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Liquid-mass method for detecting various marine biotoxins in an aquatic product

A technology of marine biology and liquid mass spectrometry, applied in the direction of measuring devices, instruments, scientific instruments, etc., can solve the problems of loss, reduce the ionization efficiency of the target, affect the detection effect, etc., and achieve the effect of reducing loss

Active Publication Date: 2019-08-20
NINGBO ACAD OF SCI & TECH FOR INSPECTION & QUARANTINE
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

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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  • Liquid-mass method for detecting various marine biotoxins in an aquatic product
  • Liquid-mass method for detecting various marine biotoxins in an aquatic product
  • Liquid-mass method for detecting various marine biotoxins in an aquatic product

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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, draw 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 method for detecting various marine biotoxins in an aquatic product. The sample of the aquatic product to be tested is extracted by using 0.1 vol% formic acid aqueous solution and acetonitrile in a classification way repeatedly, and layering is carried out to acquire upper organic phase and lower aqueous phase. The lower aqueous phase is added into an MCX-HLBseries column. Rinsing is carried out with a low proportion of methanol water. Elution is carried out with the organic phase purified by dSPE. Secondary elution is carried out with alkaline methanol.A high performance liquid chromatography-tandem mass spectrometer is used for detection after adding eluant with a dropper to bring the bottom of the meniscus to the line. An external standard methodis used for quantification to acquire the content of each component to be tested in the sample of the aquatic product to be tested. According to the invention, eight kinds of hydrophilic and lipophilic marine biotoxins can be detected at one time, and first-step liquid-mass high-throughput quantitative detection of hydrophilic and lipophilic marine biotoxins is realized.

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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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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