食品科学2017，Vol.38Issue(18)：304-309,6.DOI:10.7506/spkx1002-6630-201718047
免疫亲和净化-液相色谱-串联质谱法测定贝类中腹泻性贝类毒素
Determination of Diarrhetic Shellfish Poisons in Shellfish by Immunoaffinity Column Cleanup Coupled with Liquid Chromatography-Mass Spectrometry
摘要
Abstract
A new method using immunoaffinity chromatography (IAC) combined with liquid chromatography-tandem mass spectrometry (LC-MS/MS) was established for the determination of diarrhetic shellfish poisons (DSP) such as okadaic acid (OA), dinophysistoxin-1 (DTX1), pectenotoxin-1 (PTX1) in shellfish. Samples were extracted with 80% methanol, diluted with phosphate buffer, cleaned up by immunoaffinity chromatography, and detected by LC-MS/MS. The major parameters affecting the performance of IAC, including loading amount, washing time and elution conditions, were investigated. Detection was carried out by electrospray ionization in the negative ion mode using multiple reaction monitoring (MRM). The linear range of the analytes was 1.0–100 μg/L with correlation coefficient more than 0.996. The limit of detection (LOD) and limit of quantification (LOQ) for the analytes were calculated as 0.3 and 1.0 μg/kg, respectively. The mean recoveries of the analytes were in the range of 82.7%–94.3% with a relative standard deviation (RSD) of less than 7.61%. Therefore, the method could be used to identify and quantify diarrhetic shellfish poisons in shellfish with less matrix interference and satisfactory sensitivity.关键词
免疫亲和/液相色谱-串联质谱/腹泻性贝类毒素Key words
immunoaffinity chromatography (IAC)/liquid chromatography-tandem mass spectrometry (LC-MS/MS)/diarrhetic shellfish poison分类
轻工纺织引用本文复制引用
严忠雍,张小军,李奇富,陈思,李佩佩,祝银,刘文静..免疫亲和净化-液相色谱-串联质谱法测定贝类中腹泻性贝类毒素[J].食品科学,2017,38(18):304-309,6.基金项目
浙江省科研院所科技服务项目(2016F30020) （2016F30020）
浙江省分析测试科技计划项目(2016C37026) （2016C37026）
