摘要
建立了快速检测红鳍东方鲀肉中剧毒生物毒素河鲀毒素(Tetrodotoxin,TTX)含量的高效液相色谱-串联质谱(HPLC-MS/MS)确证方法.分析物用1%乙酸-甲醇溶液于50℃超声提取,C18和石墨化碳黑(GCB)混合粉末作为吸附剂QuEChERS净化,高速冷冻离心,上清液经尼龙-聚四氟乙烯复合膜过滤;TSK-gel Amide-80 3 μm色谱柱分离,乙腈-0.15%乙酸(含10 mmol/L乙酸铵)溶液作为流动相梯度洗脱,对滤液进行HPLC-MS/MS分析.外标法质标准曲线定量.
A simple, rapid, sensitive and cheap high performance liquid chromatography -tandemquadrupole mass spectrometric (HPLC - MS/MS) method was developed for the determination of tetro-dotoxin(Trx) that is one of the most toxic non protein small biotoxin in Fugu rubripes muscle. Theanalytes were ultrasonically extracted from homogeneous fugu muscle samples with 1% acetic acidmethanol solution at 50 ℃, purified by freezing high speed centrifugation, and succeeded cleaned byQuEChERS ( Quick, Easy, Cheap, Effective, Rugged and Safe) method using a mixture of CleanertPestiCarb and Cls as sorbent. The analyte was determined by HPLC - MS/MS using acetonitrile and0. 15% acetic acid( containing 10 mmol/L ammonium acetate)as mobile phase by gradient elution.The quantitation of TTX was performed using matrix-matched calibration curve by the external stand-ard method. Recoveries of TYX at spiked levels of 30, 50, 100 μg/kg were between 74. 0% and105.0% with relative standard deviations( RSD, n=6) not more than 11.0%. The limit of detec-tion and limit of quantitation were 10 /xg/kg and 30 μg/kg, respectively. With the advantages ofgood accuracy, repeatability, sensitivity, simplicity, economy and environment friendiness, thismethod could meet the requirements of practical analysis of Trx in fugu flesh samples.
出处
《分析测试学报》
CAS
CSCD
北大核心
2014年第5期588-593,共6页
Journal of Instrumental Analysis
基金
国家自然科学基金重点项目(41030858)
山东检验检疫局科技项目(SK201228)
关键词
河鲀毒素
红鳍东方鲀肉
液相色谱-质谱
质谱
快速提取
tetrodotoxin(Trx)
Fugu rubripes flesh
QuEChERS
high performance liquid chro-matograph - tandem quadrupole mass spectrometry (HPLC - MS/MS)
quick extraction