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,1.7μm)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0.5~100μg/L、0.5~50μg/L质量浓度范围内呈良好的线性关系,相关系数(r^2)均大于0.99,检出限(LOD,S/N≥3)为100~150μg/kg,定量下限(LOQ,S/N≥10)为300~450μg/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。
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-anh TTX,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,1.7μm)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 0.5-100μg/L for TTX and 0.5-50μg/L for 4,9-anhTTX,with their correlation coefficients(r^2)larger than 0.99.The limits of detection(LOD)and limits of quantitation(LOQ)were in the ranges of 100-150μg/kg and 300-450μg/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.
作者
王兴龙
蔡强
诸寅
保聪
桂文锋
任一平
WANG Xing-long;CAI Qiang;ZHU Yin;BAO Cong;GUI Wen-feng;REN Yi-ping(Analysis and Test Center,Yangtze Delta Region Institute of Tsinghua University,Jiaxing314000,China;Marine Animal Ecology Group,Wageningen University,Wageningen6708 WD,Holland;School of Environmental and Geographical Sciences,Shanghai Normal University,Shanghai200233,China)
出处
《分析测试学报》
CAS
CSCD
北大核心
2020年第5期640-645,共6页
Journal of Instrumental Analysis
基金
国家重点研发计划(2017YFC1601300)
研究院青年业务骨干教育培养(A类)。
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
direct dilution
tetrodotoxin
ultra high performance liquid chromatography-tandem mass spectrometry
puffer fish
nassarius
