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当前位置: 首页 > 文章 > 液相色谱-串联质谱法测定文蛤中3种腹泻性贝类毒素 安徽农业科学 2018 (34) 166-168
Position: Home > Articles > Determination of Three Diarrheal Shellfish Toxins in Clam by Liquid Chromatography-tandem Mass Spectrometry Journal of Anhui Agricultural Sciences 2018 (34) 166-168

液相色谱-串联质谱法测定文蛤中3种腹泻性贝类毒素

作  者：
张秋云;朱晓华;杨洪生;沈美芳;谭秀慧;夏莉萍
单  位：
农业农村部渔业产品质量监督检验测试中心(南京);江苏省水产质量检测中心;江苏省淡水水产研究所
关键词：
腹泻性贝类毒素;液相色谱-串联质谱;文蛤
摘  要：
[目的]以文蛤中的腹泻性贝类毒素大田软海绵酸贝类毒素(OA)、鳍藻毒素-1(DTX1)、鳍藻毒素-2(DTX2)为研究对象,建立腹泻性贝类毒素的超高效液相色谱-串联质谱(LC-MS/MS)检测方法。[方法]以文蛤样品为代表,用甲醇提取,采用碱水解将乙酰酯化的OA、DTX1、DTX2转化成游离OA、DTX1、DTX2,通过Strata-X柱净化,过膜后,用液相色谱-串联质谱测定,以基质标准曲线进行外标法定量。该试验以流动相A为水溶液(含2 mmol/L甲酸铵和1‰甲酸),流动相B为乙腈溶液(含2 mmol/L甲酸铵和1‰甲酸),流速350μL/min,柱温40℃,负离子扫描,多反应监测模式下进行定性与定量分析。[结果]3种腹泻性贝类毒在1～100μg/L关系良好,3个添加水产的回收率都在75%～90%,RSD都在3.0%～6.6%。[结论]利用此方法检测文蛤中的腹泻性贝类毒素具有灵敏度高、重复性好、操作简单的特点。回收率等均能满足日常对3种常见的腹泻性贝类毒素的检测要求。
译  名：
Determination of Three Diarrheal Shellfish Toxins in Clam by Liquid Chromatography-tandem Mass Spectrometry
作  者：
ZHANG Qiu-yun;ZHU Xiao-hua;YANG Hong-sheng;Jiangsu Fishery Quality Testing Center;Jiangsu Freshwater Fisheries Research Institute;Fishery Product Quality Supervision,Inspection and Testing Center,Ministry of Agriculture and Rural Agriculture;
单  位：
ZHANG Qiu-yun%ZHU Xiao-hua%YANG Hong-sheng%Jiangsu Fishery Quality Testing Center%Jiangsu Freshwater Fisheries Research Institute%Fishery Product Quality Supervision,Inspection and Testing Center,Ministry of Agriculture and Rural Agriculture
关键词：
Diarrhetic shellfish poisoning;;Liquid chromatography-tandem mass spectrometry;;Clam
摘  要：
[Objective]The diarrhetic shellfish toxins in field clams,Daejeon cress acid shellfish toxins,finatoxin-1 and finococcal toxin-2 were studied to establish a diarrhetic shellfish toxin by ultra performance liquid chromatography-tandem mass spectrometry method.[Method]We used the sample of scorpion as the representative,extracted with methanol,convert acetylated OA,DTX1,DTX2 into free OA,DTX1,DTX2 by alkaline hydrolysis,purified by Strata-X column,passed the membrane,and used liquid chromatography-Tandem mass spectrometry was performed and quantified by external standard method using a matrix standard curve.[Result]The three diarrhea shellfish poisons had a good relationship in the range of 1-100 μg/L,and the recovery rates of the three added aquatic products were between 75% and 90%,and the RSD was between 3.0% and 6.6%.[Conclusion]The use of this method to detect diarrhetic shellfish toxin in the scorpion had high sensitivity,good repeatability and simple operation. The recovery rate could meet the daily requirements for the detection of three common diarrheal shellfish toxins.

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