虾、海螺和蟹中麻痹性贝类毒素的 LC-FLD 和 HILIC-MS/MS 方法的精密度和重现性研究

Performance Characteristics of Refined LC-FLD and HILIC-MS/MS Methods for the Determination of Paralytic Shellfish Toxins in Shrimp, Whelk, and Crab.

机构信息

Centre for Environment, Fisheries and Aquaculture Science (Cefas), The Nothe, Weymouth, Dorset, UK.

出版信息

J AOAC Int. 2021 Aug 20;104(4):1022-1035. doi: 10.1093/jaoacint/qsab028.

DOI:10.1093/jaoacint/qsab028

PMID:33681973

Abstract

BACKGROUND

Paralytic Shellfish Poison (PSP) toxins have been reported in non-bivalve shellfish species, including crustaceans and gastropods. Routine surveillance of these species is currently conducted in parts of England. To date, detection methods have not been validated for these matrices. Validation is required to ensure the test is fit for purpose, to give greater confidence in any results generated and ultimately facilitates accreditation.

OBJECTIVE

The aim was to test and validate two independent PSP toxin detection methods previously validated for bivalve shellfish matrices, for applicability to commercial non-bivalve species of interest.

METHODS

Matrices were shrimp (Crangon crangon), common whelk (Buccinum undatum), and edible crab (Cancer pagurus). The two methods assessed were the pre-column oxidation high-performance liquid chromatography-fluorescence detection AOAC 2005.06 Official Method of analysis and an internationally validated hydrophilic interaction chromatography-tandem mass spectrometry method. Brown and white crab meat were assessed separately.

RESULTS

A refined extraction protocol was implemented with an increased solvent to sample ratio. The same extraction protocol was utilized for both methods, allowing both methods to be run simultaneously. Method sensitivity, recovery, repeatability, and method uncertainty were characterized in all matrix/toxin combinations. Overall, both methods performed similarly to that previously reported in bivalve mollusks. Acceptability of the majority of toxin/matrix combinations was evidenced through comparison of method performance characteristics against specific performance criteria, including Horwitz ratio values.

CONCLUSIONS

Both PSP toxin detection methods were found to provide acceptable performance for the monitoring of shrimp, whelk, and crab species.

HIGHLIGHTS

Two PSP toxin detection methods have been single-laboratory validated successfully for three non-bivalve shellfish species.

摘要

背景

麻痹性贝类毒素（PSP）毒素已在非双壳贝类物种中报告，包括甲壳类动物和腹足类动物。目前，在英格兰的部分地区对这些物种进行常规监测。迄今为止，尚未对这些基质进行检测方法验证。验证是必需的，以确保测试符合目的，对生成的任何结果更有信心，并最终促进认证。

目的

旨在测试和验证两种先前针对双壳贝类基质验证的独立 PSP 毒素检测方法，以确定其对商业非贝类感兴趣物种的适用性。

方法

基质为虾（Crangon crangon）、普通海螺（Buccinum undatum）和食用蟹（Cancer pagurus）。评估的两种方法是柱前氧化高效液相色谱-荧光检测 AOAC 2005.06 官方分析方法和国际上验证的亲水相互作用色谱-串联质谱法。分别评估了棕色和白色蟹肉。

结果

实施了改进的提取方案，增加了溶剂与样品的比例。两种方法均使用相同的提取方案，允许同时运行两种方法。在所有基质/毒素组合中都对方法灵敏度、回收率、重复性和方法不确定性进行了表征。总体而言，两种方法的性能与先前在双壳贝类中报告的方法相似。通过将方法性能特征与特定性能标准（包括 Horwitz 比值）进行比较，证明了大多数毒素/基质组合的可接受性。