液相色谱-串联质谱联用结合分散固相萃取法测定贝类中的软骨藻酸

[Determination of domoic acid in shellfish by liquid chromatography- tandem mass spectrometry coupled with dispersive solid phase extraction].

作者信息

Fang Li, Wu Fan, Qiu Fengmei, Yu Xinwei, Zhu Yanhua

机构信息

Key Laboratory of Health Risk Factors for Seafood of Zhejiang Province, Zhoushan Municipal Center for Disease Control and Prevention, Zhoushan 316021, China.

Wannan Medical College, School of Laboratory Medicine, Wuhu 241002, China.

出版信息

Wei Sheng Yan Jiu. 2021 Jan;50(1):116-142. doi: 10.19813/j.cnki.weishengyanjiu.2021.01.020.

DOI:10.19813/j.cnki.weishengyanjiu.2021.01.020

PMID:33517972

Abstract

OBJECTIVE

A method utilizing liquid chromatography-tandem mass spectrometry(LC-MS/MS) coupled with dispersive solid phase extraction for quantitative analysis of domoic acid in four kinds of shellfish was established.

METHODS

The sample of 0. 1 g was extracted with 25% methanol aqueous solution, the extract was purified by dispersive solid phase extraction with 50 mg HLB and 5 mg GCB, and then filtered through a PTFE membrane. The analytes were separated on a C_(18) column(100 mm×2. 1 mm, 1. 9 μm), and detected in selected reaction monitoring(SRM) mode via positive electrospray ionization. The matrix matching and external standard method was used for quantitation.

RESULTS

Domoic acid showed good linearity in the concentration range between 1. 0 ng/mL and 50. 0 ng/mL with correlation coefficients higher than 0. 9994. The detection limits of domoic acid in shellfish was 5 μg/kg. The inter-and intra-day recoveries were 91. 6%-109. 2% and 90. 9%-109. 3%, respectively. The inter-and intra-day ralitive standard deviations(RSDs) were lower than 8. 2% at spiked concentrations of 20, 50 and 100 μg/kg.

CONCLUSION

The method is accurate, fast, easy to operate, which can satisfy the requirements of public health emergency testing or routine testing.

摘要

目的

建立一种利用液相色谱 - 串联质谱法（LC-MS/MS）结合分散固相萃取技术对4种贝类中的软骨藻酸进行定量分析的方法。

方法

称取0.1 g样品，用25%甲醇水溶液提取，提取物用50 mg HLB和5 mg GCB进行分散固相萃取纯化，然后通过聚四氟乙烯（PTFE）膜过滤。分析物在C18柱（100 mm×2.1 mm，1.9 μm）上分离，采用正电喷雾电离在选择反应监测（SRM）模式下进行检测。采用基质匹配和外标法进行定量。

结果

软骨藻酸在1.0 ng/mL至50.0 ng/mL浓度范围内线性关系良好，相关系数高于0.9994。贝类中软骨藻酸的检出限为5 μg/kg。日内和日间回收率分别为91.6% - 109.2%和90.9% - 109.3%。在加标浓度为20、50和100 μg/kg时，日内和日间相对标准偏差（RSD）均低于8.2%。