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

Overview

Journal Toxins (Basel)

Publisher MDPI

Specialty Toxicology

Date 2017 Jun 30

PMID 28661471

Citations 5

Authors

Xianli Yang

Lei Zhou

Yanglan Tan

Xizhi Shi

Zhiyong Zhao

Dongxia Nie

Changyan Zhou

Hong Liu

Affiliations

Soon will be listed here.

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 -sulfo carbamoyl toxins C1 and C2, in sea shellfish. The samples were extracted by acetonitrile/water (80:20, /) 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 (² ≥ 0.9900), average recovery (81.52-116.50%), sensitivity (limits of detection (LODs): 0.33-5.52 μg·kg; limits of quantitation (LOQs): 1.32-11.29 μg·kg) 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.

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References

Mol H, Plaza-Bolanos P, Zomer P, Rijk T, Stolker A, Mulder P . Toward a generic extraction method for simultaneous determination of pesticides, mycotoxins, plant toxins, and veterinary drugs in feed and food matrixes. Anal Chem. 2008; 80(24):9450-9. DOI: 10.1021/ac801557f. View

Lawrence J, Niedzwiadek B, Menard C . Quantitative determination of paralytic shellfish poisoning toxins in shellfish using prechromatographic oxidation and liquid chromatography with fluorescence detection: collaborative study. J AOAC Int. 2006; 88(6):1714-32. View

Wang D . Neurotoxins from marine dinoflagellates: a brief review. Mar Drugs. 2008; 6(2):349-71. PMC: 2525493. DOI: 10.3390/md20080016. View

Diener M, Erler K, Christian B, Luckas B . Application of a new zwitterionic hydrophilic interaction chromatography column for determination of paralytic shellfish poisoning toxins. J Sep Sci. 2007; 30(12):1821-6. DOI: 10.1002/jssc.200700025. View

Watanabe R, Matsushima R, Harada T, Oikawa H, Murata M, Suzuki T . Quantitative determination of paralytic shellfish toxins in cultured toxic algae by LC-MS/MS. Food Addit Contam Part A Chem Anal Control Expo Risk Assess. 2013; 30(8):1351-7. DOI: 10.1080/19440049.2013.793456. View

Jansson D, Astot C . Analysis of paralytic shellfish toxins, potential chemical threat agents, in food using hydrophilic interaction liquid chromatography-mass spectrometry. J Chromatogr A. 2015; 1417:41-8. DOI: 10.1016/j.chroma.2015.09.029. View

Toyofuku H . Joint FAO/WHO/IOC activities to provide scientific advice on marine biotoxins (research report). Mar Pollut Bull. 2006; 52(12):1735-45. DOI: 10.1016/j.marpolbul.2006.07.007. View

Turrell E, Stobo L, Lacaze J, Piletsky S, Piletska E . Optimization of hydrophilic interaction liquid chromatography/mass spectrometry and development of solid-phase extraction for the determination of paralytic shellfish poisoning toxins. J AOAC Int. 2009; 91(6):1372-86. View

DellAversano C, Eaglesham G, Quilliam M . Analysis of cyanobacterial toxins by hydrophilic interaction liquid chromatography-mass spectrometry. J Chromatogr A. 2004; 1028(1):155-64. DOI: 10.1016/j.chroma.2003.11.083. View

10.

Anastassiades M, Lehotay S, Stajnbaher D, Schenck F . Fast and easy multiresidue method employing acetonitrile extraction/partitioning and "dispersive solid-phase extraction" for the determination of pesticide residues in produce. J AOAC Int. 2003; 86(2):412-31. View

11.

Wiese M, DAgostino P, Mihali T, Moffitt M, Neilan B . Neurotoxic alkaloids: saxitoxin and its analogs. Mar Drugs. 2010; 8(7):2185-211. PMC: 2920551. DOI: 10.3390/md8072185. View

12.

Boundy M, Selwood A, Harwood D, McNabb P, Turner A . Development of a sensitive and selective liquid chromatography-mass spectrometry method for high throughput analysis of paralytic shellfish toxins using graphitised carbon solid phase extraction. J Chromatogr A. 2015; 1387:1-12. DOI: 10.1016/j.chroma.2015.01.086. View

13.

DeGrasse S, Van de Riet J, Hatfield R, Turner A . Pre- versus post-column oxidation liquid chromatography fluorescence detection of paralytic shellfish toxins. Toxicon. 2011; 57(4):619-24. DOI: 10.1016/j.toxicon.2010.12.017. View

14.

DellAversano C, Hess P, Quilliam M . Hydrophilic interaction liquid chromatography--mass spectrometry for the analysis of paralytic shellfish poisoning (PSP) toxins. J Chromatogr A. 2005; 1081(2):190-201. DOI: 10.1016/j.chroma.2005.05.056. View

15.

Garrido Frenich A, Romero-Gonzalez R, Gomez-Perez M, Vidal J . Multi-mycotoxin analysis in eggs using a QuEChERS-based extraction procedure and ultra-high-pressure liquid chromatography coupled to triple quadrupole mass spectrometry. J Chromatogr A. 2011; 1218(28):4349-56. DOI: 10.1016/j.chroma.2011.05.005. View

16.

Lawrence J, Niedzwiadek B . Quantitative determination of paralytic shellfish poisoning toxins in shellfish by using prechromatographic oxidation and liquid chromatography with fluorescence detection. J AOAC Int. 2001; 84(4):1099-108. View

17.

Harju K, Rapinoja M, Avondet M, Arnold W, Schar M, Luginbuhl W . Results of a Saxitoxin Proficiency Test Including Characterization of Reference Material and Stability Studies. Toxins (Basel). 2015; 7(12):4852-67. PMC: 4690102. DOI: 10.3390/toxins7124852. View

18.

Halme M, Rapinoja M, Karjalainen M, Vanninen P . Verification and quantification of saxitoxin from algal samples using fast and validated hydrophilic interaction liquid chromatography-tandem mass spectrometry method. J Chromatogr B Analyt Technol Biomed Life Sci. 2011; 880(1):50-7. DOI: 10.1016/j.jchromb.2011.11.015. View

19.

Fernandez-Amado M, Prieto-Blanco M, Lopez-Mahia P, Muniategui-Lorenzo S, Prada-Rodriguez D . Strengths and weaknesses of in-tube solid-phase microextraction: A scoping review. Anal Chim Acta. 2016; 906:41-57. DOI: 10.1016/j.aca.2015.12.007. View

20.

Lawrence J, Menard C . Liquid chromatographic determination of paralytic shellfish poisons in shellfish after prechromatographic oxidation. J Assoc Off Anal Chem. 1991; 74(6):1006-12. View