Development and Application of Tandem LC-MS Method for the Determination of Paralytic Shellfish Poisoning Toxins for Pollution Monitoring

2011 ◽  
Vol 55-57 ◽  
pp. 51-56
Author(s):  
Xiao Ling Zhang ◽  
Bing Feng ◽  
You Qiong Cai ◽  
Hui Juan Yu
Keyword(s):  
Paralytic Shellfish Poisoning ◽  
Pollution Monitoring ◽  
Reaction Monitoring ◽  
Liquid Chromatography Mass Spectrometry ◽  
Shellfish Poisoning ◽  
Factors Affecting ◽  
Selective Determination ◽  
Paralytic Shellfish ◽  
Relative Standard

In the present study, the development of the tandem liquid chromatography-mass spectrometry (LC-MS) method for the sensitive and selective determination of eight paralytic shellfish poisoning (PSP) (GTX1, GTX2, GTX3, GTX4, GTX5, dcGTX2, dcGTX3 and dcNEO-b) toxins was investigated. Various experimental factors affecting the pretreatment and LC-MS procedures were optimzed, respectively. Using slected reaction monitoring (SRM) mode in LC-MS analysis, the acquired calibration curves were strictly linear with the value ofr2more than 0.996 for the eight targeted analyses. The obtained data expressed as relative standard deviations (RSDs), for the within-laboratory reproducibility and repeatability were less than 6.9% and 7.9%, respectively. The feasibility of the proposed method was finally validated by analyzing the eight PSPs in shellfish samples from diverse Chinese sea areas for the quality assurance of the aquatic producs and enviroment protection monitoring.

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 Optimization of Hydrophilic Interaction Liquid Chromatography/Mass Spectrometry and Development of Solid-Phase Extraction for the Determination of Paralytic Shellfish Poisoning Toxins

2008 ◽  
Vol 91 (6) ◽  
pp. 1372-1386 ◽  
Author(s):  
Elizabeth Turrell ◽  
Lesley Stobo ◽  
Jean-Pierre Lacaze ◽  
Sergey Piletsky ◽  
Elena Piletska
Keyword(s):  
Liquid Chromatography ◽  
Solid Phase ◽  
Paralytic Shellfish Poisoning ◽  
Phase Extraction ◽  
Liquid Chromatography Mass Spectrometry ◽  
Shellfish Poisoning ◽  
Hydrophilic Interaction ◽  
Paralytic Shellfish ◽  
Psp Toxins

Abstract The combination of hydrophilic interaction liquid chromatography (HILIC) and liquid chromatography/mass spectrometry (LC/MS) for the determination of paralytic shellfish poisoning (PSP) toxins has been proposed for use in routine monitoring of shellfish. In this study, methods for the detection of multiple PSP toxins [saxitoxin (STX), neosaxitoxin (NEO), decarbamoyl saxitoxin (dcSTX), decarbamoyl neosaxitoxin (dcNEO), gonyautoxins 15 (GTX1, GTX2, GTX3, GTX4, GTX5), decarbamoyl gonyautoxins (dcGTX2 and dcGTX3), and the N-sulfocarbamoyl C toxins (C1 and C2)] were optimized using single (MS) and triple quadrupole (MS/MS) instruments. Chromatographic separation of the toxins was achieved by using a TSK-gel Amide-80 analytical column, although superior chromatography was observed through application of a ZIC-HILIC column. Preparative procedures used to clean up shellfish extracts and concentrate PSP toxins prior to analysis were investigated. The capacity of computationally designed polymeric (CDP) materials and HILIC solid-phase extraction (SPE) cartridges to retain highly polar PSP toxins was explored. Three CDP materials and 2 HILIC cartridges were assessed for the extraction of PSP toxins from aqueous solution. Screening of the CDPs showed that all tested polymers adsorbed PSP toxins. A variety of elution procedures were examined, with dilute 0.01 acetic acid providing optimum recovery from a CDP based on 2-(trifluoromethyl)acrylic acid as the monomer. ZIC-HILIC SPE cartridges were superior to the PolyLC equivalent, with recoveries ranging from 70 to 112 (ZIC-HILIC) and 0 to 90 (PolyLC) depending on the PSP toxin. It is proposed that optimized SPE and HILIC-MS methods can be applied for the quantitative determination of PSP toxins in shellfish.

Application of Nanoscale Poly(divinyl-Benzene Vinylpyrrolidone) as Solid-Phase Extraction Adsorbent Prior to LC-MS-MS for the Determination of Paralytic Shellfish Poisoning Toxins in Shellfish

2011 ◽  
Vol 467-469 ◽  
pp. 2085-2090
Author(s):  
Xiao Ling Zhang ◽  
Bing Feng ◽  
You Qiong Cai ◽  
Hui Juan Yu
Keyword(s):  
Solid Phase Extraction ◽  
Solid Phase ◽  
Paralytic Shellfish Poisoning ◽  
Phase Extraction ◽  
Shellfish Poisoning ◽  
Selective Determination ◽  
Paralytic Shellfish ◽  
Divinyl Benzene ◽  
As Solid Phase

In the present study, the feasibility of the poly(divinyl-benzene vinylpyrrolidone) as solid-phase extraction (SPE) nanoscale adsorbent prior to LC-MS-MS method for the sensitive and selective determination of eight paralytic shellfish poisoning (PSP) (GTX1, GTX2, GTX3, GTX4, GTX5, dcGTX2, dcGTX3 and dcNEO-b) toxins in the shellfish was investigated. Various parameters affecting SPE efficiency including the eluent and its volume, and sample volume were studied. The application of the SPE can remove most of the ematrix interference compared with the conventional SPE procedure. By using slected reaction monitoring (SRM) mode in LC-MS-MS analysis, the acquired calibration curves were strictly linear (r2 > 0.996) for the eight targeted analyses. The feasibility of the proposed method was finally validated by quantifing the eight PSPs in the shellfish samples (scallop, Crassostrea gigas and Ruditapes philippinarum) with the satisfitory recoveries of more than 80% with RSDs less than 10%.

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.

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