Rapid Profiling and Confirmation of Azaspiracids in Edible Shellfishes by Ultra High Performance Liquid Chromatography-High Resolution Mass Spectrometry

doi:10.7506/spkx1002-6630-201404024

Abstract

Abstract:

An ultra high performance liquid chromatography-high resolution mass spectrometric method (UHPLC-LTQ/
Orbitrap) was developed for the rapid profiling and confirmation of 3 natural azaspiracids (AZAs) (AZA-1, AZA-2 and
AZA-3) in edible shellfishes including mussels, oysters, clams and scallops as well as related products. Samples were
homogeneously extracted with acetonitrile-water. The diluted supernatants were then purified with a modified QuEChERS
method. The separation was performed on an Acquity HSS T3 column (150 mm × 2.1 mm, 1.8 μm) by gradient elution with
acetonitrile in water containing 5 mmol/L ammonium acetate and 0.1% formic acid. The high-resolution mass spectrometry
was carried out by means of electrospray ionization in positive ion mode (ESI＋). The AZAs were detected by high-resolution
MS under full scan and data-dependent scan modes, respectively. The limits of quantification (LOQ, RSN > 10) were 10 μg/kg
for all the 3 AZA s. The calibration curves showed good linearity within the concentration range of 10 μg/L to 500 μg/L with
correlation coefficients (R2) more than 0.99. Shellfish samples from home and abroad were profiled and confirmed by the
established method. AZA s were found in some samples. Therefore this method is easy, sensitive, reproducible and efficient,
and can be applied to profile and confirm AZA s in edible shellfishes and related products.

Key words: azaspiracids shellfish toxins, high performance liquid chromatography-high resolution mass spectrometry, QuEChERS

CLC Number:

O657.6

HAN Shen, LIU Xin, LI Jian-hui, WANG Pei-yue, GU Jin, ZHANG Zhao-hui*. Rapid Profiling and Confirmation of Azaspiracids in Edible Shellfishes by Ultra High Performance Liquid Chromatography-High Resolution Mass Spectrometry[J]. FOOD SCIENCE, 2014, 35(4): 116-121.

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