Method for measuring three kinds of brevetoxins in shellfishes through liquid chromatography tandem mass spectrometry

A technique of tandem mass spectrometry and liquid chromatography, applied in the field of toxin detection, can solve the problems of low detection sensitivity, complicated detection method steps, and inability to detect three kinds of short dinoflagellate toxins at the same time, achieves high sensitivity, is conducive to investigation and tracking, The method is stable and reliable

Inactive Publication Date: 2018-12-14
MARINE FISHERIES RES INST OF ZHEJIANG
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Problems solved by technology

[0004] In order to solve the problems of the detection methods in the prior art with complicated steps, low detection sensitivity and the inability to detect three kinds of brevis toxins at the same time, the present invention provides a method that can improve the detection efficiency and detection sensitivity and can detect three kinds of toxins at the same time. Determination of three brevetoxins in shellfish by liquid chromatography-tandem mass spectrometry

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  • Method for measuring three kinds of brevetoxins in shellfishes through liquid chromatography tandem mass spectrometry
  • Method for measuring three kinds of brevetoxins in shellfishes through liquid chromatography tandem mass spectrometry
  • Method for measuring three kinds of brevetoxins in shellfishes through liquid chromatography tandem mass spectrometry

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Embodiment 1

[0037] A liquid chromatography tandem mass spectrometry method for the determination of three brevetoxins in shellfish, the specific steps are as follows:

[0038] a) Weigh 1.00g (accurate to 0.01g) fully homogeneous sample to be tested, place it in a 15mL centrifuge tube, add 4mL acetone, vortex for 2min, ultrasonically oscillate at room temperature for 10min, centrifuge at 5000r / min for 6min, and remove the supernatant Transfer the solution to a 50mL centrifuge tube; add 16mL water to the 50mL centrifuge tube, and ultrasonically vibrate for 0.5min to obtain the mixed solution to be purified;

[0039] b) Pipette the above mixture into the C 18 Solid-phase extraction column; after sample loading, rinse with 5mL 20% methanol aqueous solution, drain the residual liquid in the column, and discard all the above effluent, then elute with 3mL acetonitrile, collect the eluate with a 15mL centrifuge tube, Vortex for 1 min, and filter through a 0.22 μm organic phase microporous membra...

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Abstract

The invention belongs to the technical field of toxin detection, and discloses a method for measuring three kinds of brevetoxins in shellfishes through a liquid chromatography tandem mass spectrometry. Pre-processing steps are optimized from the four aspects of an extraction reagent, a solid-phase extraction column, sampling solution and eluant; and a high-efficiency liquid chromatography-tandem mass spectrometry detection method of brevetoxins in shellfishes is established. A pre-processing method in the invention is simple, high in sensitivity and good in stability, and suitable for simultaneous measurement of three kinds of brevetoxins in shellfishes; the detection method in the invention is used for quantitatively analyzing three kinds of brevetoxins in shellfishes through the liquid chromatography tandem mass spectrometry; the method is high in recovery rate and good in repeatability; the quantitation limit is up to 3.0 mu g / kg; the method is steady, reliable and high in sensitivity; current analysis detection requirements of brevetoxins are satisfied; the method has popularization and application values; and thus, marine ecological environment monitoring and survey tracking of a pollution source are easily carried out.

Description

technical field [0001] The invention relates to the technical field of toxin detection, in particular to a method for determining three brevetoxins in shellfish by liquid chromatography tandem mass spectrometry. Background technique [0002] Brevetoxin (BTX) is a type of polyether fat-soluble algae toxin, mainly produced by dinoflagellates and some algae of the genus Gymnodinosa. Brevetoxin is a macrocyclic polyether substance composed of 10 to 11 ring structures. It is a strong sodium channel activating toxin, which can bind to the target site VI of the sodium channel receptor and open the sodium channel on the excitatory membrane. , can increase the permeability of the cell membrane to sodium ions, activate voltage-gated sodium channels, produce strong cell depolarization, and cause changes in the conduction of neuromuscular excitation, so it is also called neurotoxin. The brevetoxin is thermally stable, making its elimination half-life in shellfish and other organisms as...

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02
CPCG01N30/02
Inventor 严忠雍张小军陈思方益
Owner MARINE FISHERIES RES INST OF ZHEJIANG
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