CONSTRUCTION OF A FINGERPRINT TRACEABILITY TECHNIQUE BASED ON UPLC-Q-EXACTIVE MS FOR THE CHARACTERIZATION OF PARALYTIC SHELLFISH POISON
The risk of paralytic shellfish toxins(PSTs)in bivalves has become a serious food safety issue of common concern worldwide,especially due to the difficulty how to trace the positive products to their farming area.We developed a fingerprinting technique based on ultra-performance liquid chromatography-quadrupole electrostatic field orbitrap high-resolution mass spectrometry(UPLC-Q-Exactive MS)to identify the regional characteristics of paralytic shellfish toxin by simulating the changes of toxin in three species of toxic algae after exposure to Mytilus galloprovincialis and establishing a pretreatment and chromatographic mass spectrometry method for the characteristic fingerprint samples.Results show that the extraction of the compounds by acetonitrile/methanol/acetone(1∶1∶1,v∶v∶v),positive ion mode m/z 100～600 using C8 column and positive ion mode m/z 600～1 500 using amide column was efficient and stable,covering 40.4％of the compounds in total.And the toxin components of the M.galloprovincialis were metabolically transformed after ingestion of different toxin-producing algae.The principal component analysis(PCA)and orthogonal signal correction partial least squares-discriminant analysis(OPLS-DA)models were conducted to identify 13 fingerprints for the identification of algae species,and the cross-validation accuracy of the Fisher discriminant model was 88.9％.The fingerprint traceability technology based on UPLC-Q-Exactive MS on M.galloprovincialis traits has preliminarily realized the retrospect searching for accountable algae species of the poison contamination to shellfish,and shall be promoted in the cultures of mussel or other shellfish.
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