超高效液相色谱-串联质谱法测定贝类中6种脂溶性贝类毒素  

Analysis for 6 kinds of liposoluble shellfish toxins from shellfish products by UPLC-MS/MS

作　　者：曹杰[1] 朱峰[2] 王强[3] 张春玲[1] 和佳鸳 徐虹[1] CAO Jie;ZHU Feng;WANG Qiang;ZHANG Chun-ling;HE Jia-yuan;XU Hong(Zhenjiang Municipal Center for Disease Control and Prevention,Jiangsu Zhenjiartg 212000,China;不详)

机构地区：[1]镇江市疾病预防控制中心,江苏镇江212000 [2]江苏省疾病预防控制中心 [3]江苏大学医学院

出　　处：《江苏预防医学》2020年第3期241-244,共4页Jiangsu Journal of Preventive Medicine

基　　金：镇江市重点研发计划(社会发展)项目(SH2018017)

摘　　要：目的建立贝类中6种脂溶性贝类毒素(蛤毒素PTX2、虾夷扇贝毒素YTX和HYTX、鳍藻毒素DTX1和DTX2、大田软海绵酸OA)超高效液相色谱-串联质谱(UPLC-MS/MS)方法,并监测2019年江苏省市售贝类中6种脂溶性贝类毒素的残留。方法样品经甲醇提取,采用Waters BEH C18色谱柱(2.1mm×100mm,1.7μm)分离,以乙腈-0.01%氨水体系为流动相,在电喷雾离子源多反应监测模式下检测,外标法定量。根据2019年江苏省食品安全风险监测方案要求,在全省5个城市采集104份贝类产品进行检测。结果6种脂溶性贝类毒素PTX2、YTX、HYTX、OA、DTX1和DTX2在质量浓度范围为2.0~40.0ng/ml线性关系良好,相关系数(r)均>0.99,方法检出限范围为10~20μg/kg,在贝类样品基质(扇贝)中6种脂溶性贝类毒素低、中、高浓度水平平均回收率为60.1%~125.0%,相对标准偏差(RSD)为1.4%~8.6%。2019年采集的104份贝类样品中,HYTX、OA、DTX1和DTX2均未检出,PTX2和YTX各检出1份,检出值均未超出欧盟制订的最大残留限量。结论建立的方法灵敏、准确、稳定,适用于贝类中6种脂溶性贝类毒素的测定。Objective To establish an ultra-performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS)method for the determination of 6 liposoluble shellfish toxins(PTX2,YTX,HYTX,OA,DTX1 and DTX2);to investigate toxin contamination status of 6 liposoluble shellfish toxins from market sold shellfish products in Jiangsu province in 2019.Methods Samples were extracted by methanol and separated by Waters BEH C18 column(2.1 mm×100 mm,1.7μm).Acetonitrile-0.01% ammonia water system was used as mobile phase.Determination was performed under multiple reaction monitoring mode.External standard method was used for quantitative analysis.According to the requirements of the food safety risk monitoring program of Jiangsu province in 2019,a total of 104 shellfish products from five cities of Jiangsu province were collected for analysis.Results The linear relationship of 6 kinds of liposoluble shellfish toxinswas good in mass concentration range of 2.0-40.0 ng/ml,all the linear correlation coefficient was more than 0.99.The LOD was in the range of 10-20μg/kg,the average recovery rates of low,medium and high concentration levels were from 60.1% to 125.0%,RSDs were from 1.4% to 8.6%.For 104 shellfish samples collected in 2019,HYTX,OA,DTX1 and DTX2 were not detected,while PTX2 and YTX were detected in 1 sample and the detection values were lower than the maximum residue limits defined by the European Union.Conclusion The results show that the method is sensitive,accurate and stable,which is suitable for the determination of 6 liposoluble shellfish toxins in shellfish.

关 键 词：食品安全 风险监测 超高效液相色谱-串联质谱法 脂溶性贝类毒素 贝类 

分 类 号：R113[医药卫生—公共卫生与预防医学]