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High performance liquid chromatography mass spectrometry detecting method of 16 fat soluble saxitoxins in shellfish meet

A shellfish toxin and detection method technology, applied in measuring devices, instruments, scientific instruments, etc., can solve the problems of inability to clearly distinguish the composition of shellfish toxins, high detection limits for animal welfare, and no tissue differences, and achieve overall recovery. The effect of high rate, saving of organic solvent and processing time, excellent qualitative function

Inactive Publication Date: 2013-02-13
YELLOW SEA FISHERIES RES INST CHINESE ACAD OF FISHERIES SCI
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Problems solved by technology

The fat solubility of LPs leads to the elimination half-life of such toxins in shellfish and other organisms as long as tens of days or even months, and the distribution in shellfish muscle, viscera and other tissues does not have significant tissue differences, and heating, Conventional processing methods such as microwaves reduce the moisture content in aquatic products and lead to higher concentrations of toxins. Therefore, the potential harm of such toxins to consumers is more difficult to prevent, and it has become an important concern for developed countries such as the European Union to formulate trade and technical barriers point
The existing detection technology is mainly the mouse biological method, which has problems such as animal welfare and high detection limit, and cannot clearly distinguish the components of shellfish toxins. Although mass spectrometry detection technology has also begun to be used for the detection of shellfish toxins, the detection types are relatively single , or the pretreatment method needs to be further improved

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  • High performance liquid chromatography mass spectrometry detecting method of 16 fat soluble saxitoxins in shellfish meet
  • High performance liquid chromatography mass spectrometry detecting method of 16 fat soluble saxitoxins in shellfish meet
  • High performance liquid chromatography mass spectrometry detecting method of 16 fat soluble saxitoxins in shellfish meet

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[0029] The technical scheme of the present invention will be further explained below by the examples, but the protection scope of the present invention is not limited by any form of the examples

[0030] A liquid-mass spectrometry detection method for 16 fat-soluble shellfish toxins in shellfish, the steps of which are as follows:

[0031] (1) Sample treatment: Weigh 2 g of sample into a 15 mL stoppered centrifuge tube, add 5 mL of methanol, vortex mix for 1 min, and ultrasonically extract for 5 min. Centrifuge at 4000r / min for 5min, and take the supernatant into a 10mL graduated glass centrifuge tube. Add 5 mL of methanol to the residue, repeat the extraction once, and combine the two extracts. Blow nitrogen gas at 40°C to about 1 mL, add 3 mL of water, vortex mix, and sonicate for 1 min, and wait for purification.

[0032] (2) Purification: activate Strata with 1mL methanol and 1mL 30% methanol aqueous solution in sequence TM -X solid phase extraction column, inject the e...

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Abstract

The invention discloses a high performance liquid chromatography mass spectrometry detecting method of 16 fat soluble saxitoxins in shellfish meet. The detecting method comprises the following steps of: processing a sample, purifying, testing the condition, qualitatively testing and quantitatively testing. According to the detecting method, methanol is adopted for extraction and a solid phase extraction column is adopted for purification so as to carry out the synchronous detection on the 16 fat soluble saxitoxins in the shellfish meet. The method is simple and convenient to operate, good in a purification effect, high in overall recycling rate and strong in reconstruction capability, and meanwhile an organic solvent and the processing time are saved, and the pretreatment process of the sample is simplified.

Description

technical field [0001] The invention relates to a method for detecting fat-soluble shellfish toxins, in particular to a method for detecting 16 kinds of fat-soluble shellfish toxins in shellfish by liquid mass spectrometry Background technique [0002] Marine biotoxins (shellfish toxins) specifically refer to a large class of small molecule toxic chemicals that are mainly produced by marine toxic microalgae or microorganisms, can be enriched in marine organisms, especially bivalve molluscs, and are harmful to other organisms including humans. substance. For these biological toxins, researchers initially divided them into six categories based on the symptoms of poisoning they caused: Paralytic Shellfish Poisoning (PSP), Diarrhetic Shellfish Poisoning (DSP), Neurotoxicity Neurotoxic Shellfish Poisoning (NSP), Amnesic Shellfish Poisoning (ASP), Ciguatera Fish Poisoning (CFP), and blue-green algae toxins. However, with the deepening of research, new types of biological toxins ...

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Application Information

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IPC IPC(8): G01N30/02G01N30/60
Inventor 谭志军吴海燕郭萌萌李兆新王联珠翟毓秀
Owner YELLOW SEA FISHERIES RES INST CHINESE ACAD OF FISHERIES SCI
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