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1.
Food Chem ; 298: 125011, 2019 Nov 15.
Article in English | MEDLINE | ID: mdl-31261011

ABSTRACT

A scallop midgut gland certified reference material, NMIJ CRM 7520-a, was developed for validation and quality assurance during the inspection of shellfish for diarrhetic shellfish toxins. The candidate material was prepared by using naturally-toxic and nontoxic boiled midgut glands spiked with okadaic acid (OA). The homogeneity and stability of the material were found to be appropriate. For the characterization of OA and dinophysistoxin-1 (DTX1), nine participants were involved in a co-laboratory study based on the Japanese Official Testing Method, where the compounds were assayed by liquid chromatography-tandem mass spectrometry following alkaline hydrolysis. The analytical values were obtained by the standard addition method with a standard spiking solution calibrated using the standard-solution certified reference materials OA and DTX1. The certified concentrations with expanded uncertainties (coverage factor k = 2, approximate 95% confidence interval) were determined to be (0.205 ±â€¯0.061) mg/kg for OA and (0.45 ±â€¯0.11) mg/kg for DTX1.


Subject(s)
Diarrhea/complications , Marine Toxins/analysis , Pectinidae/chemistry , Pyrans/analysis , Shellfish/analysis , Animals , Calibration , Chromatography, Liquid , Humans , Intestines/chemistry , Marine Toxins/standards , Marine Toxins/toxicity , Okadaic Acid/analysis , Pyrans/standards , Pyrans/toxicity , Reference Standards , Shellfish Poisoning/complications , Tandem Mass Spectrometry
5.
Environ Toxicol Pharmacol ; 48: 7-16, 2016 Dec.
Article in English | MEDLINE | ID: mdl-27716534

ABSTRACT

Saxitoxin (STX) and its analogs, the paralytic shellfish toxins (PSTs), are a group of potent neurotoxins well known for their role in acute paralytic poisoning by preventing the generation of action potentials in neuronal cells. They are found in both marine and freshwater environments globally and although acute exposure from the former has previously received more attention, low dose extended exposure from both sources is possible and to date has not been investigated. Given the known role of cellular electrical activity in neurodevelopment this pattern of exposure may be a significant public health concern. Additionally, the presence of PSTs is likely to be an ongoing and possibly increasing problem in the future. This review examines the neurodevelopmental toxicity of STX, the risk of extended or repeated exposure to doses with neurodevelopmental effects, the potential implications of this exposure and briefly, the steps taken and difficulties faced in preventing exposure.


Subject(s)
Environmental Exposure/adverse effects , Neurotoxicity Syndromes/etiology , Saxitoxin/toxicity , Shellfish Poisoning/complications , Water Pollutants, Chemical/toxicity , Animals , Climate Change , Cyanobacteria/genetics , Cyanobacteria/growth & development , Dinoflagellida/genetics , Dinoflagellida/growth & development , Dose-Response Relationship, Drug , Environmental Exposure/analysis , Fresh Water/chemistry , Humans , Ion Channels/antagonists & inhibitors , Molecular Structure , Neurotoxicity Syndromes/metabolism , Saxitoxin/administration & dosage , Saxitoxin/analysis , Saxitoxin/chemistry , Seawater/chemistry , Time Factors , Water Pollutants, Chemical/administration & dosage , Water Pollutants, Chemical/analysis , Water Pollutants, Chemical/chemistry
6.
J AOAC Int ; 99(5): 1151-62, 2016 Sep.
Article in English | MEDLINE | ID: mdl-27524810

ABSTRACT

Okadaic acid (OA) and its analogs dinophysistoxins-1 (DTX1) and -2 (DTX2) are lipophilic polyethers produced by marine dinoflagellates. These toxins accumulate in shellfish and cause diarrhetic shellfish poisoning (DSP) in humans. Regulatory testing of shellfish is essential to safeguard public health and for international trade. Certified reference materials (CRMs) play a key role in analytical monitoring programs. This paper presents an overview of the interdisciplinary work that went into the planning, production, and certification of calibration-solution CRMs for OA, DTX1, and DTX2. OA and DTX1 were isolated from large-scale algal cultures and DTX2 from naturally contaminated mussels. Toxins were isolated by a combination of extraction and chromatographic steps with processes adapted to suit the source and concentration of each toxin. New 19-epi-DSP toxin analogs were identified as minor impurities. Once OA, DTX1, and DTX2 were established to be of suitable purity, solutions were prepared and dispensed into flame-sealed glass ampoules. Certification measurements were carried out using quantitative NMR spectroscopy and LC-tandem MS. Traceability of measurements was established through certified external standards of established purity. Uncertainties were assigned following standards and guidelines from the International Organization for Standardization, with components from the measurement, stability, and homogeneity studies being propagated into final combined uncertainties.


Subject(s)
Diarrhea/complications , Marine Toxins/analysis , Okadaic Acid/analysis , Pyrans/analysis , Reference Standards , Shellfish Poisoning/complications , Animals , Calibration , Chromatography, Liquid/standards , Humans , Magnetic Resonance Spectroscopy/standards , Shellfish , Tandem Mass Spectrometry/standards
7.
J AOAC Int ; 99(5): 1163-72, 2016 Sep.
Article in English | MEDLINE | ID: mdl-27546874

ABSTRACT

Okadaic acid (OA) and its analogs, dinophysistoxins-1 (DTX1) and -2 (DTX2) are lipophilic biotoxins produced by marine algae that can accumulate in shellfish and cause the human illness known as diarrhetic shellfish poisoning (DSP). Regulatory testing of shellfish is required to protect consumers and the seafood industry. Certified reference materials (CRMs) are essential for the development, validation, and quality control of analytical methods, and thus play an important role in toxin monitoring. This paper summarizes work on research and development of shellfish tissue reference materials for OA and DTXs. Preliminary work established the appropriate conditions for production of shellfish tissue CRMs for OA and DTXs. Source materials, including naturally incurred shellfish tissue and cultured algae, were screened for their DSP toxins. This preliminary work informed planning and production of a wet mussel (Mytilus edulis) tissue homogenate matrix CRM. The homogeneity and stability of the CRM were evaluated and found to be fit-for-purpose. Extraction and LC-tandem MS methods were developed to accurately certify the concentrations of OA, DTX1, and DTX2 using a combination of standard addition and matrix-matched calibration to compensate for matrix effects in electrospray ionization. The concentration of domoic acid was also certified. Uncertainties were assigned following standards and guidelines from the International Organization for Standardization. The presence of other toxins in the CRM was also assessed and information values are reported for OA and DTX acyl esters.


Subject(s)
Diarrhea/complications , Marine Toxins/analysis , Okadaic Acid/analysis , Pyrans/analysis , Shellfish Poisoning/complications , Animals , Calibration , Chromatography, Liquid/standards , Humans , Molecular Conformation , Reference Standards , Shellfish , Tandem Mass Spectrometry/standards
8.
Wei Sheng Yan Jiu ; 35(4): 435-8, 2006 Jul.
Article in Chinese | MEDLINE | ID: mdl-16986518

ABSTRACT

OBJECTIVE: Paralytic shellfish poisoning (PSP) and diarrhetic shellfish poisoning (DSP) in 7 species of economical shellfishes were analyzed for 1 year, which collected from Huangsha seafood market of Guangzhou from Apr, 2004 to Mar, 2005. METHODS: The levels of PSP and DSP in bivalves were determined with mouse bioassay of AOAC. The risk assessment of PSP and DSP in bivalves was conducted according to FAO and Chinese Administration Organization of Fish Culture and Seaport. RESULTS: PSP was detected in 2 species of the shellfishes assayed and DSP was found out in 6 species. The content of PSP was lower than 4MU/g tissue, whereas the level of PSP in glands was higher than in muscles. DSP toxin was detected in 36 samples of 6 species, what is more, DSP level in 10 samples exceeded the safety threshold. The levels in PSP and DSP of bivalves were all higher in spring and winter with some characteristic of season. CONCLUSION: The results suggested that PSP in economical shellfish in Guangzhou market was lower, and shellfish was safe to eat in term of the PSP level if glands were discarded, but DSP contamination in bivalves was severe. It is essential to detect and assess the risk of DSP and PSP in bivalves from seafood market in the future.


Subject(s)
Food Contamination/analysis , Marine Toxins/analysis , Saxitoxin/analysis , Shellfish Poisoning/complications , Shellfish/analysis , Animals , Bivalvia , Diarrhea/etiology , Marine Toxins/poisoning , Mice , Paralysis/chemically induced , Paralysis/etiology , Saxitoxin/poisoning
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