A mussel tissue certified reference material for multiple phycotoxins. Part 4: certification (original) (raw)

A mussel tissue certified reference material for multiple phycotoxins. Part 1: design and preparation

Analytical and Bioanalytical Chemistry, 2011

The development of multi-analyte methods for lipophilic shellfish toxins based on liquid chromatography-mass spectrometry permits rapid screening and analysis of samples for a wide variety of toxins in a single run. To ensure accuracy of results, validated methods and appropriate certified reference materials (CRMs) are required. CRMs are essential for accurate instrument calibration, for assessing the complete analytical method from sample extraction to data analysis, and for verifying trueness. However, CRMs have hitherto only been available for single toxin groups.

Accumulation of phycotoxins in the mussel Mytilus galloprovincialis from the Central Adriatic Sea

Croatica chemica acta, 2006

Sažetak Surveys of DSP (Diarrheic Shellfish Poisoning) toxin profiles in the mussel Mytilus galloprovincialis from coastal waters of the central Adriatic Sea, over the years 1995 to 2001, demonstrate that incidents of shellfish toxicity in this area are dominated by the occurrence of okadaic acid (OA) and a PTX derivative, 7-epi-pectenotoxin-2-seco acid (7-epi-PTX-2SA). Toxin composition and the relative ratio of toxic components in shellfish is in correlation with the occurrence of DSP producing organisms from the Dinophysis species along with ...

Mussels Based Food Supplements: Evaluation of Emerging Marine Toxins is a Necessary Evil

Food supplements containing mussel extracts are becoming popular in human diet, providing high levels of proteins, omega-3 polyunsaturated fatty acid (PUFAs), iodine and carbohydrates. Besides the beneficial effects and bioactives that mussel may yield, it is vital to consider the potential harmful phycotoxins that can be present in mussel extracts and marine dietary supplements. Recently, we have detected for the first time the marine toxin 13-desmethyl spirolide C in food supplements containing green lipped mussels of Perna canaliculus at levels up to 98 µg/kg. In this work, we provide new data about the presence of pinnatoxin-G (trace amounts) in the dietary supplements intended for human consumption after the analysis of the green lipped mussel powder by UPLC-MS/MS. Moreover, the status of microalgae phycotoxin contaminants is also assessed in these products and in animal dietary supplements which contained 13-desmethyl spirolide C at levels up to 39 µg/kg. The mechanism of action of spirolides and pinnatoxins is associated with the blockage of the muscarinic and nicotinic receptors (mAChR and nAChR) on the nervous system. Despite the fact that human intoxications have not been reported, it is important to identify the impact of such toxins on public health since dietary products constitute an important part of the global market.

Occurrence of phycotoxins in marine shellfish other than bivalve molluscs: an update

The specifications from the European "hygiene package" directive consider all commercial shellfish. The sanitary safety of bivalve molluscs, the most widely consumed group, is tested by national monitoring plans. Marine shellfish other than bivalves, such as gastropods, echinoderms and tunicates, also represent a food safety concern and are currently not considered in most European monitoring plans. In order to estimate the relevance of implementing maximal limits for these types of products, an update of data regarding their ability to accumulate phycotoxins was requested by the French regulatory authorities. Marine gastropods are the family that is the best documented for contamination data, other than bivalves. The ability of some gastropod species to accumulate phycotoxins (mainly PSP toxins) is clearly demonstrated. However, there is limited information available about some other species such as Buccinum undatum or Littorina littorea, which are commonly consumed in Fr...

Phycotoxins: Chemistry and Biochemistry

2007

Monitoring brevetoxins during a Gymnodinium breve red tide: comparison of sodium channel specific cytotoxicity assay and mouse bioassay for determination of neurotoxic shellfish toxins in shellfish extracts.

LC-MS/MS Analysis of the Emerging Toxin Pinnatoxin-G and High Levels of Esterified OA Group Toxins in Galician Commercial Mussels

Toxins, 2019

The occurrence of marine harmful algae is increasing worldwide and, therefore, the accumulation of lipophilic marine toxins from harmful phytoplankton represents a food safety threat in the shellfish industry. Galicia, which is a commercially important EU producer of edible bivalve mollusk have been subjected to recurring cases of mussel farm closures, in the last decades. This work aimed to study the toxic profile of commercial mussels (Mytilus galloprovincialis) in order to establish a potential risk when ingested. For this, a total of 41 samples of mussels farmed in 3 Rías (Ares-Sada, Arousa, and Pontevedra) and purchased in 5 local markets were analyzed by liquid chromatography tandem mass spectrometry (LC-MS/MS). Chromatograms showed the presence of okadaic acid (OA), dinophysistoxin-2 (DTX-2), pectenotoxin-2 (PTX-2), azaspiracid-2 (AZA-2), and the emerging toxins 13-desmethyl spirolide C (SPX-13), and pinnatoxin-G (PnTX-G). Quantification of each toxin was determined using their own standard calibration in the range 0.1%-50 ng/mL (R2 > 0.99) and by considering the toxin recovery (62-110%) and the matrix correction (33-211%). Data showed that OA and DTX-2 (especially in the form of esters) are the main risk in Galician mollusks, which was detected in 38 samples (93%) and 3 of them exceeded the legal limit (160 µg/kg), followed by SPX-13 that was detected in 19 samples (46%) in quantities of up to 28.9 µg/kg. Analysis from PTX-2, AZA-2, and PnTX-G showed smaller amounts. Fifteen samples (37%) were positive for PTX-2 (0.7-2.9 µg/kg), 12 samples (29%) for AZA-2 (0.1-1.8 µg/kg), and PnTX-G was detected in 5 mussel samples (12%) (0.4 µg/kg-0.9 µg/kg). This is the first time Galician mollusk was contaminated with PnTX-G. Despite results indicating that this toxin was not a potential risk through the mussel ingestion, it should be considered in the shellfish safety monitoring programs through the LC-MS/MS methods. Keywords: lipophilic marine toxin levels; Galician mussels; liquid chromatography-mass spectrometry (LC-MS/MS); new emerging toxins Key Contribution: First description of the emerging pinnatoxins in mollusk from the Atlantic coast of Spain. Presence of high levels of OA group toxins in Galician commercial mussels analyzed by liquid chromatography tandem mass spectrometry.

Recent developments in the detection of phycotoxins

Over the past seven years, methods available for the detection of phycotoxins have been extensively reviewed in a number of international expert committees, such as the consultations organised by FAO/IOC/WHO and EFSA, as well as by individual scientists. These reviews have shown that the methods available have severe limitations for the use in official control, either due to their limited scope and detection capability or due to a lack of calibration standards, reference materials and validation efforts. The present review focuses on recent developments in the detection of phycotoxins in several areas of applied research. Not being able to exhaustively describe all recent developments, the review focussed on three areas of interest to the authors: (i) detection of ultra-trace amounts of toxins, (ii) metabolism of toxins and their localisation in biological tissues, and (iii) approaches to detect unknown toxins or analogues of known toxins.

Recent developments in the analysis of phycotoxins by liquid chromatography-mass spectrometry

… in Perspective at the Turn of the Century. …, 2001

The combination of liquid chromatography and mass spectrometry (LC-MS) is a powerful tool for the detection and quantitation of phycotoxins in plankton and shellfish at trace levels, the identification of new toxins, the investigation of toxin production by plankton, and the study of toxin metabolism in shellfish. Progress in development of LC-MS as a "universal" toxin analysis method for the comprehensive analysis of a wide range of toxins is now described. Two basic methods have been developed: lipophilic toxins are separated on a reversed phase column using gradient elution, while the paralytic shellfish poisoning (PSP) toxins are separated on a hydrophilic interaction LC column using isocratic elution.