超高效液相色谱-三重四级杆串联质谱法测定贝类中的9种脂溶性贝类毒素  

Determination of 9 kinds of liposoluble shellfish toxins in shellfish by ultra high performance liquid chromatography-triple quadruple mass spectrometry

作　　者：陈颖[1] 白欣[1] 宋月[1] CHEN Ying;BAI Xin;SONG Yue(Dalian Center for Disease Control arwl Prevention,Dalian,Liaoning 116021,China)

机构地区：[1]大连市疾病预防控制中心,辽宁大连116021

出　　处：《中国卫生检验杂志》2019年第1期22-25,共4页Chinese Journal of Health Laboratory Technology

摘　　要：目的建立多种贝类食品中9种脂溶性贝类毒素超高效液相色谱-三重四级杆串联质谱法。方法经甲醇提取,以Waters BEH C18(2. 1 mm×10 mm,1. 7μm)为分离柱,乙腈和0. 01%氨水溶液为流动相梯度洗脱,超高效液相色谱-串联四级杆质谱仪测定,外标法定量,测得游离态毒素;采用碱水解将酯化毒素转化为游离态,以Waters BEH C18(2. 1 mm×10 mm,1. 7μm)为分离柱,乙腈和0. 01%氨水溶液为流动相梯度洗脱,超高效液相色谱-串联四级杆质谱仪测定,外标法定量,测得毒素总量。结果本法在2. 5 ng/ml～50 ng/ml内呈良好线性关系,相关系数> 0. 99,最低检出限为10μg/kg～20μg/kg,相对标准偏差<15%。结论本方法操作简单、灵敏度高、重现性好,且具有较好的选择性和特异性,能满足贝类食品中9种脂溶性贝类毒素同时检测的要求,为贝类食物中毒诊断提供了可靠的实验室依据。Objective To establish a method for 9 kinds of liposoluble shellfish toxins in shellfish by ultra high performance liquid chromatography-triple quadruple mass spectrometry(UPLC-MS/MS).Methods After methanol extraction,the free toxin was separated with a Waters BEH C18 column (2.1mm×10mm,1.7μm)and detected with triple quadruple mass spectrometer and quantified by the external standard method;acetonitrile and 0.01% ammonia solution were used as mobile phases.The analytes were detected with triple quadruple mass spectrometer and quantified by the external standard method.The total amount of toxin was measured.Results The method showed a good linear relationship within 2.5ng/ml -50ng/ml with the correlation coefficient greater than 0.99.The detection limits were within 10g/kg -20μg/kg,with relative deviations less than 15%.Conclusion The method is simple,sensitive,and selective.It can be used for the detection of 9kinds of liposoluble shellfish toxins in shellfish and provide reliable basis for laboratory.

关 键 词：超高效液相色谱-三重四级杆串联质谱法 贝类 脂溶性贝类毒素 

分 类 号：O657.63[理学—分析化学]