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Method for detecting diarrheal shellfish poison in shellfish meat by utilizing liquid chromatography-mass spectrometry (LC-MS)

A technology of diarrheal shellfish poisoning and LC/MS, applied in the field of LC/MS, can solve the problems of complex and time-consuming sample pretreatment, and achieve the effects of saving extraction time, simplifying the extraction process and fast sample preprocessing.

Inactive Publication Date: 2011-10-12
SHANGHAI OCEAN UNIV
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Problems solved by technology

[0005] The technical problem to be solved by the present invention is to overcome the defects that OA and DTX1 in the existing liquid chromatography-mass spectrometry detection DSP are complicated sample pretreatment and time-consuming, and use ultra-high performance liquid chromatography quadrupole time-of-flight mass spectrometry (UPLC / Q-TOFMS) to quickly detect OA and DTX1, and use it in the detection of commercially available seafood shellfish, in order to provide a fast and efficient detection technology for toxic red tide research and food safety inspection

Method used

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Examples

Experimental program
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Effect test

Embodiment

[0040] 1. Weigh 2g of homogenized clam muscle sample that has been artificially fed with poison, put it in a 10ml centrifuge tube, and add 3mL of 80% methanol aqueous solution. Vortex for 1 min, ultrasonically oscillate for 1 min, and centrifuge at 4°C (5000 r / min, 5 min). The supernatant was transferred to another clean centrifuge tube, and the residue was extracted once more according to the above method. Combine the supernatants, add 5mL of n-hexane, vortex mix, let stand and discard the upper layer of n-hexane, repeat once, combine the methanol phase, add 1ml of water (containing 0.2% acetic acid), repeat the extraction twice with 6ml of chloroform , combined the chloroform phase of the lower layer, and fed N with a rotary evaporator 2 Evaporate to dryness to remove the organic phase, redissolve the residue with HPLC grade methanol, and dilute to 1ml (equivalent to 2g muscle / ml). Centrifuge at high speed (10000r / min, 10min) or pass through a 0.22μm filter membrane, and w...

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Abstract

The invention provides the rapid extraction procedures of the DSP in a shellfish sample aiming at the problems of complicated sample pretreatment, great workload, high cost and great time consumption in the existing liquid chromatography-mass spectrometry (LC-MS) technique for detecting a DSP (Digital Signal Processor). In the method provided by the invention, the UP LC / Q-TOFMS (Flight Mass Spectrometry) detection in the LC-MS technique are utilized and the UP LC / Q-TOFMS detection is used for the actual detection of merchant marine shellfish, thereby providing an effective and accurate detection technique for poisonous red tide research and food safety inspection.

Description

technical field [0001] The invention relates to a liquid-mass spectrometry technique, in particular to a liquid-mass spectrometry technique (UPLC-MS) for detecting diarrheal shellfish poisoning in shellfish meat. Background technique [0002] Harmful red tides have broken out in many countries in the world, and marine shellfish can enrich red tide algae toxins in their bodies and cause harm to humans and animals through the food chain. Extensive surveys have shown that bivalve molluscs in China have been polluted by red tide algal toxins, among which diarrheal shellfish poisoning (DSP) is relatively common. DSP is a kind of fat-soluble natural compound produced by some species of toxic red tide algae Dinophysis and Prorocentrum. Its main components are okadaic acid (OA) and dinotoxin DTX1. OA and DTX1 are tumor-promoting factors that are genotoxic and can lead to the formation of DNA adducts. If the content of OA and DTX1 in shellfish liver exceeds 2μg / g and 1.8μg / g respec...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/72G01N30/36G01N30/06
Inventor 饶涛何培民唐晨汪卿贾睿胡乐琴冯子慧
Owner SHANGHAI OCEAN UNIV
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