分析化学2026，Vol.54Issue(1)：113-124,12.DOI:10.19756/j.issn.0253-3820.251174
贝类中软骨藻酸及其异构体的高效液相色谱-串联质谱分析方法及应用
Development and Application of High-Performance Liquid Chromatography-Tandem Mass Spectrometry for Analysis of Domoic Acid and Its Isomers in Shellfish
摘要
Abstract
Domoic acid(DA)is the principal neurotoxin responsible for amnesic shellfish poisoning(ASP),and exhibits escalating prevalence in China's coastal ecosystems with widespread contamination by DA and its structural isomers.To enhance regulatory control of these contaminants,an high-performance liquid chromatography-tandem mass spectrometry(HPLC-MS/MS)method for detection of DA and its isomers was developed and validated through optimization of sample preparation and chromatographic conditions.The samples were extracted with 50.0%(V/V)aqueous methanol,cleaned up using Bond Elut SAX solid-phase extraction cartridges,volume-adjusted,and filtered through 0.22 μm aqueous-phase membranes.Chromatographic separation employed a Luna C18(2)-HST 100A column(100 mm×2 mm,2.5 μm)with gradient elution(Mobile phase A:1% formic acid in water;Mobile phase B:1% formic acid in acetonitrile).Method validation demonstrated that the recoveries were 77.69%–115.84%(Relative standard deviations were 1.65%–8.96%),inter-batch recoveries were 79.39%–110.43%(RSD 1.04%–8.07%,n=6)across four shellfish matrices,with good linearity(R2≥0.999)and high sensitivity(LOD/LOQ:0.1/0.3 μg/kg).Analysis results of coastal shellfish samples of Shandong Province in 2023 revealed universal DA/isomer detection during July to September,with DA constituting 92.9%,88.7% and 89.1% of total analogs,respectively.Risk assessment results indicated negligible dietary exposure across age demographics(THQ<0.1),indicating no consumption risk.This robust methodology enabled accurate quantification of DA isomers,providing a vital monitoring framework for China's coastal regions.关键词
软骨藻酸/液相色谱-质谱联用法/贝类/风险评估Key words
Domoic acid/Liquid chromatography-tandem mass spectrometry/Shellfish/Risk assessment引用本文复制引用
徐希震,吴海燕,孙宏业,赵紫璇,谭志军,郑关超..贝类中软骨藻酸及其异构体的高效液相色谱-串联质谱分析方法及应用[J].分析化学,2026,54(1):113-124,12.基金项目
国家自然科学基金项目(Nos.42306162,32472451,42276219)、山东省自然科学基金青年项目(No.ZR2023QC148)、中国水产科学研究院基本科研业务费项目(Nos.2023TD76,2023TD28)和国家现代农业(贝类)产业技术体系专项资金项目(No.CARS-49)资助. Supported by the National Natural Science Foundation of China(Nos.42306162,32472451,42276219),the Youth Natural Science Foundation of Shandong Province(No.ZR2023QC148),the Central Public-Interest Scientific Institution Basal Research Fund,CAFS(Nos.2023TD76,2023TD28)and the Earmarked Fund for CARS(No.CARS-49). （Nos.42306162,32472451,42276219）
