Improvement in detection limits for the determination of paralytic shellfish poisoning toxins in shellfish tissues using capillary electrophoresis/electrospray mass spectrometry and discontinuous buffer systems

1994 ◽  
Vol 66 (20) ◽  
pp. 3436-3446 ◽  
Author(s):  
S. J. Locke ◽  
P. Thibault
Keyword(s):  
Mass Spectrometry ◽  
Capillary Electrophoresis ◽  
Electrospray Mass Spectrometry ◽  
Detection Limits ◽  
Paralytic Shellfish Poisoning ◽  
Shellfish Poisoning ◽  
Paralytic Shellfish

Assessment of a Semiquantitative Liquid Chromatography- Fluorescence Detection Method for the Determination of Paralytic Shellfish Poisoning Toxin Levels in Bivalve Molluscs from Great Britain

2014 ◽  
Vol 97 (2) ◽  
pp. 492-497 ◽  
Author(s):  
Andrew D Turner ◽  
Monika Dhanji-Rapkova ◽  
Clothilde Baker ◽  
Myriam Algoet
Keyword(s):  
Great Britain ◽  
Fluorescence Detection ◽  
Detection Method ◽  
Reference Method ◽  
Paralytic Shellfish Poisoning ◽  
Official Method ◽  
Shellfish Poisoning ◽  
Bivalve Molluscs ◽  
Paralytic Shellfish

Abstract AOAC Official Method 2005.06 precolumn oxidation LC-fluorescence detection method has been used for many years for the detection and quantitation of paralytic shellfish poisoning (PSP) toxins in bivalve molluscs. After extensive single- and multiple-laboratory validation, the method has been slowly gaining acceptance worldwide as a useful and practical tool for official control testing. In Great Britain, the method has become routine since 2008, with no requirement since then for reverting back to the bioassay reference method. Although the method has been refined to be semiautomated, faster, and more reproducible, the quantitation step can be complex and time-consuming. An alternative approach was developed to utilize the qualitative screening results for generatinga semiquantitative results assessment. Data obtained over 5 years enabled the comparison of semiquantitative and fully quantitative PSP results in over 15 000 shellfish samples comprising eight different species showed that the semiquantitative approach resulted in over-estimated paralytic shellfish toxin levels by an average factor close to two in comparison with the fully quantified levels. No temporal trends were observed in the data or relating to species type, with the exception of surf clams. The comparison suggested a semiquantitative threshold of 800 μg saxitoxin (STX) eq/kg should provide a safe limitfor the determination of samples to be forwarded to full quantitation. However, the decision was taken to halve this limit to include an additional safety factor of 2, resulting in the use of a semiquantitative threshold of 400 μg STX eq/kg. Implementation of the semiquantitative method into routine testing would result in a significant reduction in the numbers of samples requiring quantitation and have a positive impact on the overall turnaround of reported PSP results. The refined method would be appropriate for any monitoring laboratory faced with high throughput requirements.

scholarly journals Proficiency Testing of Eight French Laboratories in Using the AOAC Mouse Bioassay for Paralytic Shellfish Poisoning: Interlaboratory Collaborative Study

2000 ◽  
Vol 83 (2) ◽  
pp. 305-310 ◽  
Author(s):  
Martial LeDoux ◽  
Sherwood Hall ◽  
Madeleine Bohec ◽  
Bernard Charron ◽  
Magali Esnault ◽  
...  
Keyword(s):  
Water Solution ◽  
Collaborative Study ◽  
Paralytic Shellfish Poisoning ◽  
Mouse Bioassay ◽  
Shellfish Poisoning ◽  
Paralytic Shellfish ◽  
Relative Standard ◽  
Standard Solution ◽  
Overall Performance

Abstract In an interlaboratory study, 8 French laboratories were tested for their proficiency in using the AOAC mouse bioassay for paralytic shellfish poisoning (PSP). Each laboratory received 1 saxitoxin (STX) standard solution, 1 STX acidified water solution for determination of the titer, 1 noncontaminated shellfish sample, 1 naturally contaminated shellfish sample, and 2 shellfish samples spiked, respectively, at low (152.8 μg STX/100 g meat) and moderate (334.7 μg STX/100 g meat) levels. All samples were analyzed in duplicate. Mean recoveries were 35.1% for the low level and 46.6% for the moderate level. Relative standard deviations (RSD) for within-laboratory variations (repeatability) ranged from 5.4 to 9.8%; RSD for between-laboratory variations (reproducibility) varied from 7.8 to 39.6%, depending on STX level. On the basis of overall performance, all 8 participating laboratories were proficient in their use of the AOAC mouse bioassay.

scholarly journals Microbiological and Marine Biotoxins Contamination of Raw Bivalve Molluscs Commercially Available in Poland

2012 ◽  
Vol 56 (4) ◽  
pp. 563-568 ◽  
Author(s):  
Remigiusz Pomykała ◽  
Mirosław Michalski ◽  
Artur Jóźwik ◽  
Jacek Osek
Keyword(s):  
Vibrio Parahaemolyticus ◽  
Paralytic Shellfish Poisoning ◽  
Shellfish Poisoning ◽  
Bivalve Molluscs ◽  
E Coli ◽  
Marine Biotoxins ◽  
Amnesic Shellfish Poisoning ◽  
Paralytic Shellfish ◽  
Coagulase Positive Staphylococci

Abstract The study was carried out on live bivalve molluscs available on Polish market. Microbiological tests were performed for the presence of Salmonella sp., Vibrio parahaemolyticus, spore-forming anaerobe bacteria, and coagulase-positive Staphylococcus sp., and for the enumeration of Escherichia coli. ELISA was used for the determination of marine biotoxins, paralytic shellfish poisoning (PSP), amnesic shellfish poisoning (ASP), and diarrhoeic shellfish poisoning (DSP). Microbiological examinations were performed according to ISO and Polish Standards. Salmonella sp. was not detected in any sample tested. Coagulase-positive staphylococci were identified in 9.0% of the samples. V. parahaemolyticus was isolated from 17.0% of mussels. Shellfish were highly contaminated by anaerobes, which were isolated from 68.0% of the samples. The number of E. coli ranged from <2.0 x 101 up to >1.8 x 104 MPN/100 g. The majority of mussels were free from the marine biotoxins tested or contained them bellow the permitted level. The analysis of microbiological and toxicological status of raw bivalve molluscs available on Polish market indicates that they are generally safe for the consumers.

scholarly journals Quantitative Determination of Paralytic Shellfish Poisoning Toxins in Shellfish by Using Prechromatographic Oxidation and Liquid Chromatography with Fluorescence Detection

2001 ◽  
Vol 84 (4) ◽  
pp. 1099-1108 ◽  
Author(s):  
James F Lawrence ◽  
Barbara Niedzwiadek
Keyword(s):  
Quantitative Determination ◽  
Oxidation Reaction ◽  
Solid Phase ◽  
Paralytic Shellfish Poisoning ◽  
Phase Extraction ◽  
Shellfish Poisoning ◽  
Paralytic Shellfish ◽  
Cleanup Procedure ◽  
Psp Toxins

Abstract The prechromatographic oxidation LC method developed by Lawrence [J. Assoc. Off. Anal. Chem. 74, 404–409(1991)] for the determination of paralytic shellfish poisoning (PSP) toxins has been tested for the quantitative determination of PSP toxins in shellfish. All aspects of the method were studied and modified as necessary to improve its performance for routine regulatory purposes. The chromatographic conditions were changed to shorten analysis time. The oxidation reaction was tested for repeatability and the influence of the s ample matrix on quantitation. An important part of the study was to quantitatively evaluate an ion exchange (-COOH) cleanup step using disposable solid-phase extraction cartridges that separated the PSP toxins into 3 distinct groups for quantitation, namely the C toxins, the GTX toxins, and the saxitoxin group. The cleanup step was very simple and used increasing concentrations of aqueous NaCl for elution of the toxins. The C toxins were not retained by the cartridges and thus were eluted unretained with water. The GTX toxins (GTX1 to GTX6 as well as dcGTX2 and dcGTX3) eluted from the cartridges with 0.05M NaCl while the saxitoxin group (saxitoxin, neosaxitoxin, and dcsaxitoxin) required 0.3M NaCl for elution. Each fraction was analyzed by LC after oxidation with periodate or peroxide. All of the compounds could be separated and quantitatively determined in spiked samples of mussels, clams, and oysters. The nonhydroxylated toxins could be quantitated at concentrations as low as about 0.02 μg/g (2 μg/100 g) of tissue while the hydroxylated toxins could be quantitated at concentrations as low as about 0.1 μg/g (10 μg/100 g). Average recoveries of the toxins through the complete cleanup procedure were 85%or greater for spiked extracts of oysters and clams and greater than 73%for mussels.

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