高效液相色谱-串联质谱法测定福建省中北部海域贝类中的软骨藻酸

Determination of domoic acid in shellfish by high performance liquid chromatography-tandem mass spectrometry in the central-north sea areas of Fujian Province

近年来,我国沿海赤潮灾害频发,食用贝类造成的中毒事件时有发生,对贝类毒素的分析研究越来越重要。为此,本研究探究高效液相色谱-串联质谱法(HPLC-MS/MS)测定失忆性贝类毒素软骨藻酸(Domoic acid,DA)的方法条件,并进行验证。结果表明,1)DA在0.5~25.0μg/L范围内线性关系良好,定量限为5μg/kg,平均回收率为68.7%~92.4%,日内相对标准偏差在5.4%~8.4%之间(n=6),日间相对标准偏差在3.9%~5.1%之间(n=6)。2)采用该方法检测2020—2021年福建省中北部海域主要养殖贝类中的DA,结果显示:(1)136个贝类样品中有27个样品检出DA,检出率19.9%,其中福州连江县、宁德福鼎市和莆田北岸区检出率较高,达到40%及以上;(2)2021年4—6月整体检出率呈逐渐递增趋势(0%~41.5%);(3)136个样品中DA主要在花蛤、牡蛎和贻贝中检出,检出率为13.6%~35.7%,缢蛏、鲍和扇贝中均未检出。本方法具有快速、高效、高灵敏度和高准确度等优点,适用于贝类中软骨藻酸的日常检测和监控,对加强贝类风险管控具有重要意义。

In recent years,red tide disasters occur frequently in coastal areas of China,and poisoning incidents caused by eating shellfish occur from time to time.In this study,the conditions for determination of domoic acid(DA)by high performance liquid chromatography-tandem mass spectrometry(HPLC-MS/MS)were investigated and verified.The results showed as follows:1)The linear range of DA was 0.5~25.0μg/L,the limit of quantitation was 5μg/kg,the average recoveries were 68.7%~92.4%,the intra-day relative standard deviation was 5.4%~8.4%(n=6),and the inter-day relative standard deviation was 3.9%~5.1%(n=6);2)The method was used to detect DA in main cultured mollusks in the central and northern waters of Fujian Province from 2020 to 2021.(1)DA was detected in 27 samples of 136 shellfish samples,with a detection rate of 19.9%.Among them,the detection rate in Lianjiang County of Fuzhou City,Fuding City of Ningde City and Putian City Bei'an District was higher,reaching 40%or more.(2)From April to June 2021,the overall detection rate showed an increasing trend(0%~41.5%).(3)Among 136 samples,DA was mainly detected in clams,oyster and mussel with the detection rate ranging from 13.6%to 35.7%.Abalone and scallop were not detected.This method had the advantages of rapid,high efficiency,high sensitivity and high accuracy,and was suitable for the daily detection and monitoring of domoic acid in shellfish,which was of great significance for strengthening the risk control of shellfish.