Development of liquid chromatography-mass spectrometric methods for verification of paralytic shellfish poisoning toxins in complex matrices related to environmental contamination and human exposure

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http://urn.fi/URN:NBN:fi-fe201902286671
Title: Development of liquid chromatography-mass spectrometric methods for verification of paralytic shellfish poisoning toxins in complex matrices related to environmental contamination and human exposure
Author: Pettersson, Annette
Contributor: University of Helsinki, Faculty of Science
Publisher: Helsingin yliopisto
Date: 2019
Language: eng
URI: http://urn.fi/URN:NBN:fi-fe201902286671
http://hdl.handle.net/10138/299769
Thesis level: master's thesis
Discipline: Analyyttinen kemia
Abstract: Paralytic shellfish poisoning toxins belong to a group of marine biotoxins that can cause severe food poisoning. The marine biotoxins have highly varying properties, such as molecular weight, solubility and toxicity. They accumulate into shellfish during harmful algal blooms. The global fish industry monitors sea food prior to releasing them to the market to ensure the safety of consumers, and permitted levels of marine biotoxins are regulated worldwide. Possible bioterrorism use of marine biotoxins is a concern to the governments due to their high toxicity and availability. The main emphasis in this thesis is on paralytic shellfish poisoning toxins, saxitoxin and its analogues. Saxitoxin is listed under the Chemical Weapons Convention. The paralytic shellfish poisoning toxin analogues share physico-chemical properties such as solubility, but they differ highly from each other in toxicity. The most toxic analogues of paralytic shellfish poisoning toxins are the Saxitoxin and Neosaxitoxin. The toxicity of the paralytic shellfish poisoning toxins is due to the blocking of the voltage gated sodium channels, which is a reversible process. The symptoms of paralytic shellfish poisoning can be numbness, weakness and even paralysis, which can lead to respiratory failure. The paralytic shellfish poisoning can be lethal and there is no antidote. A new liquid chromatography- tandem mass spectrometric method using multiple reaction monitoring was developed. Several different hydrophilic interaction liquid chromatography type analysis columns were compared. A liquid chromatography- high resolution mass spectrometric analysis methods using full scan and product ion scan were developed for several of the paralytic shellfish poisoning toxin analogues. The limit of detection and limit of quantification for Saxitoxin analyzed with the high resolution mass spectrometry method were 0.2 ng/ml and 0.7 ng/ml respectively. In average the detection and quantification limits obtained with the high resolution mass spectrometry were around ten times better than the values obtained using triple quadrupole mass spectrometry. New sample preparation methods were developed for four different matrices (mussel, urine, milk and juice) applying solid phase extraction as the primary sample clean-up technique to be used in proficiency tests. Proficiency test samples analyzed during this thesis contained mussel, urine and unknown saxitoxin samples. The proficiency test samples were analyzed using three different chromatography-based analysis techniques to determine the presence of paralytic shellfish poisoning toxins. A comparison was done between the developed triple quadrupole mass spectrometric method, high resolution mass spectrometric method and a standardized fluorescence detection method.


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