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Toxins 2017, 9(7), 206; doi:10.3390/toxins9070206

Development and Validation of a Liquid Chromatography-Tandem Mass Spectrometry Method Coupled with Dispersive Solid-Phase Extraction for Simultaneous Quantification of Eight Paralytic Shellfish Poisoning Toxins in Shellfish

1
Institute for Agro-food Standards and Testing Technology, Laboratory of Quality & Safety Risk Assessment for Agro-products (Shanghai), Ministry of Agriculture, Shanghai Academy of Agricultural Sciences, Shanghai 201403, China
2
School of Marine Sciences, Ningbo University, Ningbo 315211, China
3
Key Laboratory of Food Safety Research, Institute for Nutritional Sciences, Shanghai Institutes for Biological Sciences, Chinese Academy of Sciences, Shanghai 200031, China
4
Shanghai Municipal Center for Disease Control and Prevention, Shanghai 200336, China
*
Authors to whom correspondence should be addressed.
Received: 26 April 2017 / Revised: 18 June 2017 / Accepted: 27 June 2017 / Published: 29 June 2017
(This article belongs to the Section Marine and Freshwater Toxins)
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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. View Full-Text
Keywords: paralytic shellfish poisoning (PSP) toxins; LC-MS/MS; dispersive solid-phase extraction (dSPE); saxitoxin paralytic shellfish poisoning (PSP) toxins; LC-MS/MS; dispersive solid-phase extraction (dSPE); saxitoxin
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Yang, X.; Zhou, L.; Tan, Y.; Shi, X.; Zhao, Z.; Nie, D.; Zhou, C.; Liu, H. Development and Validation of a Liquid Chromatography-Tandem Mass Spectrometry Method Coupled with Dispersive Solid-Phase Extraction for Simultaneous Quantification of Eight Paralytic Shellfish Poisoning Toxins in Shellfish. Toxins 2017, 9, 206.

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