scholarly journals Analysis of paralytic shellfish toxins using high-field asymmetric waveform ion mobility spectrometry with liquid chromatography-mass spectrometry

2015 ◽  
Vol 407 (9) ◽  
pp. 2473-2484 ◽  
Author(s):  
Daniel G. Beach ◽  
Jeremy E. Melanson ◽  
Randy W. Purves
Toxins ◽  
2020 ◽  
Vol 12 (6) ◽  
pp. 398
Author(s):  
Jiangbing Qiu ◽  
Elliott J. Wright ◽  
Krista Thomas ◽  
Aifeng Li ◽  
Pearse McCarron ◽  
...  

Paralytic shellfish toxins (PSTs) are a complex class of analogs of the potent neurotoxin saxitoxin (STX). Since calibration standards are not available for many PSTs, including C-11 hydroxyl analogs called M-toxins, accurate quantitation by liquid chromatography–mass spectrometry (LC-MS) can be challenging. In the absence of standards, PSTs are often semiquantitated using standards of a different analog (e.g., STX), an approach with a high degree of uncertainty due to the highly variable sensitivity between analytes in electrospray ionization. Here, relative molar response factors (RMRs) were investigated for a broad range of PSTs using common LC-MS approaches in order to improve the quantitation of PSTs for which standards are unavailable. First, several M-toxins (M1-M6, M9 and dcM6) were semipurified from shellfish using preparative gel filtration chromatography and quantitated using LC-charged aerosol detection (LC-CAD). The RMRs of PST certified reference materials (CRMs) and M-toxins were then determined using selective reaction monitoring LC-MS/MS and full scan LC-high-resolution MS (LC-HRMS) methods in positive and negative electrospray ionization. In general, RMRs for PSTs with similar chemical structures were comparable, but varied significantly between subclasses, with M-toxins showing the lowest sensitivity. For example, STX showed a greater than 50-fold higher RMR than M4 and M6 by LC-HRMS. The MS instrument, scan mode and polarity also had significant impacts on RMRs and should be carefully considered when semiquantitating PSTs by LC-MS. As a demonstration of their utility, the RMRs determined were applied to the semiquantitation of PSTs in contaminated mussels, showing good agreement with results from calibration with CRMs.


2001 ◽  
Vol 114 (23) ◽  
pp. 10270-10277 ◽  
Author(s):  
Roger Guevremont ◽  
David A. Barnett ◽  
Randy W. Purves ◽  
Larry A. Viehland

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