Abstract
In this study, a high-performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) method was developed for simultaneous determination of eight paralytic shellfish poisoning (PSP) toxins, including saxitoxin (STX), neosaxitoxin (NEO), gonyautoxins (GTX1–4) and the N-sulfo carbamoyl toxins C1 and C2, in sea shellfish. The samples were extracted by acetonitrile/water (80:20, v/v) with 0.1% formic and purified by dispersive solid-phase extraction (dSPE) with C18 silica and acidic alumina. Qualitative and quantitative detection for the target toxins were conducted under the multiple reaction monitoring (MRM) mode by using the positive electrospray ionization (ESI) mode after chromatographic separation on a TSK-gel Amide-80 HILIC column with water and acetonitrile. Matrix-matched calibration was used to compensate for matrix effects. The established method was further validated by determining the linearity (R2 ≥ 0.9900), average recovery (81.52–116.50%), sensitivity (limits of detection (LODs): 0.33–5.52 μg·kg−1; limits of quantitation (LOQs): 1.32–11.29 μg·kg−1) and precision (relative standard deviation (RSD) ≤ 19.10%). The application of this proposed approach to thirty shellfish samples proved its desirable performance and sufficient capability for simultaneous determination of multiclass PSP toxins in sea foods.
Highlights
The paralytic shellfish poisoning (PSP) toxins are potent neurotoxins produced by toxic algae in red tide [1,2] and further accumulated in shellfish [3,4]
A joint report by the Food and Agriculture Organization (FAO), the World Health Organization (WHO) and the International Oceanographic Commission of United Nations Educational, Scientific and Cultural Organization (IOC) has recommended a derived guidance level of 170 or 110 μg STXequ·kg−1 based on the consumption of 250 or 380 g shellfish meat by adults [9], and a level of 75 μg STXequ·kg−1 based on 400 g feed size was suggested [10]
For reversed-phase LC, acetonitrile and methanol are commonly used as organic phase, while acetonitrile was considered for better resolution than methanol in some of the previous reports [22]
Summary
The paralytic shellfish poisoning (PSP) toxins are potent neurotoxins produced by toxic algae in red tide [1,2] and further accumulated in shellfish [3,4]. They are known for causing severe food poisoning by intake of contaminated shellfish or other seafood [5]. These naturally produced toxins show thermal stability and cannot be destroyed even under normal heating. A joint report by the Food and Agriculture Organization (FAO), the World Health Organization (WHO) and the International Oceanographic Commission of United Nations Educational, Scientific and Cultural Organization (IOC) has recommended a derived guidance level of 170 or 110 μg STXequ·kg−1 based on the consumption of 250 or 380 g shellfish meat by adults [9], and a level of 75 μg STXequ·kg−1 based on 400 g feed size was suggested [10]
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