CAJ | 학술논문

建立了海洋生物中河豚毒素的免疫亲和柱净化-液相色谱-串联质谱分析方法。采用1%乙酸-甲醇提取样品,提取液通过磷酸盐缓冲液稀释,调节至pH 7~8,经免疫亲和柱富集和净化后,LC-MS/MS测定,外标法定量。在ACQUITY UPLC BEH Amide亲水柱上进行分离,流动相为乙腈和含有0.1%甲酸的5 mmol/L乙酸铵溶液,梯度洗脱,电喷雾正离子多反应模式监测。河豚毒素在0.3~20.0μg/L线性范围内,相关系数大于0.997,定量限为0.3μg/kg,回收率为88.7%~102.3%,相对标准偏差2.0%~6.4%。本方法重现性好、灵敏度高,适用于海洋生物中河豚毒素的测定。
건립료해양생물중하돈독소적면역친화주정화-액상색보-천련질보분석방법。채용1%을산-갑순제취양품,제취액통과린산염완충액희석,조절지pH 7~8,경면역친화주부집화정화후,LC-MS/MS측정,외표법정량。재ACQUITY UPLC BEH Amide친수주상진행분리,류동상위을정화함유0.1%갑산적5 mmol/L을산안용액,제도세탈,전분무정리자다반응모식감측。하돈독소재0.3~20.0μg/L선성범위내,상관계수대우0.997,정량한위0.3μg/kg,회수솔위88.7%~102.3%,상대표준편차2.0%~6.4%。본방법중현성호、령민도고,괄용우해양생물중하돈독소적측정。
A method was developed for the determination of tetrodotoxin in marine organisms by high perfor-mance liquid chromatography-mass spectrometry with immunoaffinity column. The samples were extracted with 1% acetic acid methanol solution and diluted with phosphate buffer at pH 7-8. After cleaned up by immuno-affinity column, the samples were analyzed by LC-MS/MS and quantitatively determined by external standard method. The chromatographic separation was performed on an ACQUITY UPLC BEH Amide column with gradient elution by using acetonitrile and 5 mol/L ammonium acetate solution containing 0. 1% formic acid as mobile phase. Detection was carried out by electrospray positive ionization mass spectrometry in the multiple reaction monitoring mode. Linear ranges of TTX was in the range of 0. 3 -20. 0 μg/L with correlation coeffi-cient more than 0. 997. The quantification limit of the method was 0. 3 μg/kg. The recoveries of standard addition for tetrodotoxin were 88. 7%-102. 3%, and the relative standard deviation was 2. 0%-6. 4%. The method could be used to identify and quantify tetrodotoxin in marine organisms with satisfactory reproducibility and sensitivity.