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直接稀释/超高效液相色谱-串联质谱法测定河豚鱼与织纹螺中2种河豚毒素
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作者单位
王兴龙,蔡强,诸寅,保聪,桂文锋,任一平 1.浙江清华长三角研究院分析测试中心2.瓦赫宁根大学海洋动物生态组
3.上海师范大学环境与地理科学学院
 
基金项目:国家重点研发计划(2017YFC1601300);研究院青年业务骨干教育培养(A类)
中文摘要:建立了直接稀释/超高效液相色谱-串联质谱测定河豚鱼与织纹螺中2种河豚毒素TTX和4,9-anh TTX的方法。样品经乙酸-甲醇(1∶99)溶液提取,高速离心,上清液用80%(体积分数)甲醇水溶液稀释和过滤后直接进样分析。以0.5 mmol/L甲酸铵的0.1%甲酸水溶液-0.1% 甲酸乙腈溶液为流动相,采用梯度洗脱方式在ACQUITY BEH Amide色谱柱(100 mm×2.1 mm,1.7 μm)上分离,以电喷雾离子源正离子模式(ESI+)扫描,多反应监测(MRM)模式采集,外标法定量。TTX和4,9-anhTTX分别在0.5~100 μg/L、0.5~50 μg/L质量浓度范围内呈良好的线性关系,相关系数(r2)均大于0.99,检出限(LOD,S/N≥3)为100~150 μg/kg,定量下限(LOQ,S/N≥10)为300~450 μg/kg。在河豚鱼、织纹螺基质中,3 个浓度水平下的加标回收率为75.4%~96.8%,日内相对标准偏差(RSD)为2.3%~9.5%,日间RSD为5.3%~9.2%。该方法简便、高效、节约成本,适用于河豚鱼、织纹螺中2 种河豚毒素的快速准确检测。
中文关键词:直接稀释  河豚毒素  超高效液相色谱-串联质谱  河豚鱼  织纹螺
 
Experimental Techniques and MethodsAnalysis of Two Kinds of Tetrodotoxins in Puffer Fish and Nassarius by Ultra High Performance Liquid Chromatography-Tandem Mass Spectrometry with Direct Dilution Approach
Abstract:An ultra high performance liquid chromatography-tandem mass spectrometric(UPLC-MS/MS) method was established for the determination of two tetrodotoxins(TTXs),eg TTX and 4,9 anhTTX,in puffer fish and nassarius with a direct dilution technique.Samples were extracted with acetic acid-methanol(1∶99,by volume).After centrifuged and diluted by 80% methanol solution,the extract was separated on an ACQUITY BEH Amide(100 mm×2.1 mm,1.7 μm) column by gradient elution,with 0.1% formic acid solution containing 05 mmol/L ammonium formate-0.1% formic acid acetonitrile solution as mobile phases,analyzed in ESI+ mode under multiple reaction monitoring(MRM) mode and quantified by external standard method.There were good linear relationships in the range of 0.5-100 μg/L for TTX and 0.5-50 μg/L for 4,9 anhTTX,with their correlation coefficients(r2) larger than 0.99.The limits of detection(LOD) and limits of quantitation(LOQ) were in the ranges of 100-150 μg/kg and 300-450 μg/kg,respectively.Recoveries at three spiked levels ranged from 75.4% to 96.8%,with intra-day relative standard deviations(RSD) and inter-day RSD of 2.3%-9.5% and 5.3%-9.2%,respectively.The method was simple and high sensitive,and was suitable for the determination of two TTXs in puffer fish and nassarius.
Key Words:direct dilution  tetrodotoxin  ultra high performance liquid chromatography-tandem mass spectrometry  puffer fish  nassarius
引用本文:王兴龙,蔡强,诸寅,保聪,桂文锋,任一平.直接稀释/超高效液相色谱-串联质谱法测定河豚鱼与织纹螺中2种河豚毒素[J].分析测试学报,2020,39(5):640-645.
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