Detection Technology And Application Of A Variety Of Shellfish Toxins In Bivalve Shellfish

With the fast development of coastal aquaculture in C hina and the wastewater of urban industrial and domestic sewage flow into the sea, eutrophication of the sea lead to the frequent occurrence of red tide. Overproduction plankton exacerbated the increase of marine biotoxins, Shellfish toxin generated by the shellfish ingesting of toxic algae or symbiosising with seaweed, these toxins accumulate in shellfish. Its damage has feature of sudden and universality. Because of its high toxicity, fast response and has no suitable antidote, brought many difficulties to the prevention and treatment. C hina has not yet established a comprehensive shellfish toxin detection security system, liquid chromatography(HPLC) and liquid chromatography-mass spectrometry(LC-MS/MS) has advantages of high sensitivity, accuracy and precision. They have a huge potential for analysis and detection of toxins in shellfish.By optimizing the chromatographic conditions, MS conditions, pre-treatment step, established LC-MS/MS analysis method to analyze diarrhetic shellfish poisoning, use mobile phase of alkaline conditions to improve peak shape, use hydrolysis pretreatment step to make DTX3 releases OA, DTX1, DTX2 three kinds of diarrhetic shellfish po isoning. By optimizing solvent extraction, SPE elution conditions to increase the recovery rate and sensitivity. Average recovery rate is 82.5%~96.3%, the relative standard deviations is 3.4%~9.3%, the detection limit can reach 0.2 ng/g. Established LC-MS/MS analysis method to analyze neurotoxic shellfish poisoning, use mobile phase of acidic conditions to improve peak shape. By optimizing solvent extraction, SPE elution conditions to increase the recovery rate and sensitivity. Average recovery rate is 80.6%~92.5%, the relative standard deviations is 4.2%~7.2%, the detection limit can reach 0.4 ng/g. Established HPLC analysis method to analyze amnesic shellfish poisoning, including two pre-treatment technology. Developed and verified the quechers pretreatment methods. By optimizing solvent extraction, matrix with standard to increase the recovery rate and sensitivity. Compared quechers to another pre-treatment method their advantages and disadvantages.This study established three analysis methods of three kinds of shellfish toxins. Compared to the earlier mice method has advantage of higher accuracy, and LC-MS/MS has higher sensitivity and accuracy than the current shellfish toxin detection standards. Provide data support for promoting the establish of shellfish detection and monitoring system. The average recoveries of the two methods are 91.3% ~ 92.8% and 75.5%-87.3%, the relative standard deviations is 2.7%~4.3% and 3.3%~5.1%, the detection limit is 1.8 μg/g and 0.3 μg/g.