| Article ID | Journal | Published Year | Pages | File Type |
|---|---|---|---|---|
| 1202903 | Journal of Chromatography A | 2014 | 8 Pages |
•tITP-CE with C4D detection for the separation of paralytic shellfish toxins (PSTs).•A 10-fold reduction in detection limits than without ITP, but in the presence of 25 mM sodium chloride in the sample.•Demonstrated by application to extracts from contaminated mussels and compared to HPLC data.•This is the first report of tITP being used in combination with CE-C4D.
The accumulation of paralytic shellfish toxins (PSTs) in contaminated shellfish is a serious health risk making early detection important to improve shellfish safety and biotoxin management. Capillary electrophoresis (CE) has been proven as a high resolution separation technique compatible with miniaturization, making it an attractive choice in the development of portable instrumentation for early, on-site detection of PSTs. In this work, capillary zone electrophoresis (CZE) with capacitively coupled contactless conductivity detector (C4D) and UV detection were examined with counter-flow transient isotachophoresis (tITP) to improve the sensitivity and deal with the high conductivity sample matrix. The high sodium concentration in the sample was used as the leading ion while l-alanine was used as the terminating electrolyte (TE) and background electrolyte (BGE) in which the toxins were separated. Careful optimization of the injected sample volume and duration of the counter-flow resulted in limit of detections (LODs) ranging from 74.2 to 1020 ng/mL for tITP-CZE-C4D and 141 to 461 ng/mL for tITP-CZE-UV, an 8–97 fold reduction compared to conventional CZE. The LODs were adequate for the analysis of PSTs in shellfish samples close to the regulatory limit. Intra-day and inter-day repeatability values (percentage relative standard deviation, n = 3) of tITP-CZE-C4D and tITP-CZE-UV methods for both migration time and peak height were in the range of 0.82–11% and 0.76–10%, respectively. The developed method was applied to the analysis of a contaminated mussel sample and validated against an Association of Official Analytical Chemists (AOAC)-approved method for PSTs analysis by high performance liquid chromatography (HPLC) with fluorescence detection (FLD) after pre-column oxidation of the sample. The method presented has potential for incorporation in to field-deployable devices for the early detection of PSTs on-site.
