超高效液相色谱荧光法检测贝类中三种高毒性麻痹性贝毒  

Analysis of three paralytic shellfish poisoning toxins with high toxicity in shellfish by UPLC with fluorescence detection

作　　者：张晓玲[1] 杨桥[1] 惠芸华[1] 冯兵[1] 马丽艳[1] 于慧娟[1] 

机构地区：[1]中国水产科学研究院东海水产研究所,上海200090

出　　处：《海洋渔业》2012年第3期337-341,共5页Marine Fisheries

基　　金：中央级公益性科研院所基本科研业务费专项资金资助项目(2008M17)

摘　　要：建立灵敏可靠的麻痹性贝类毒素(PSP)检测技术是保障我国贝类水产品质量安全的有力手段。本研究选取3-(2-呋喃甲酰基)-喹啉-2-羰醛(FQ)为荧光衍生试剂,利用超高效液相色谱(UPLC)和柱前衍生荧光检测技术,建立了贝类中3种高毒性PSP毒素成分(STX、GTX1及NEO)的检测方法,对影响荧光衍生效率和色谱分离效果的各主要实验因素分别进行了优化。结果表明,在优化后的最佳实验条件下,3种PSP毒素成分线性方程的相关系数(r)均大于0.998,保留时间(tm)及峰面积(PA)的日内及日间精密度RSD值分别小于3.1%和5.6%,当信噪比(S/N)等于3时,检测限范围为7～14μg.kg-1,样品加标回收率为82%～92%,RSD值小于5.2%。该方法灵敏、稳定且可靠,可用于贝类中三种高毒性PSP毒素成分的日常分析检测。Establishing sensitive and reliable analytical methods for inspection on paralytic shellfish poisoning（PSP） toxins in shellfish foods is an effective mean to ensure the quality and safety of aquatic products in China.In this paper,the suitability of the ultra performance liquid chromatography（UPLC） and precolumn derivatization for the analysis of three PSP toxins（STX,GTX1 and NEO） with high toxicity in shellfish was investigated by choosing 3-（2-furoyl）quinoline-2-carboxaldehyde（FQ） as the derivatization reagent.Various parameters affecting the derivatization reaction and the UPLC separation were respectively optimized.Under the optimal conditions,the correlation coefficients（r） of three calibration equations were more than 0.998,the relative standard deviations（RSD） values of the intra-day and inter-day precision for the retention time and peak area of the three targeted analyses were less than 3.1% and 5.6%,respectively.The limits of detection（LOD） were 7-14 μg·kg-1.The spiked recoveries were determined as in the range of 82-92% with the RSDs value less than 5.2%.The proposed method has proven sensitive and reliable,and can be used for the routine analysis of three PSP toxins in shellfish.

关 键 词：麻痹性贝毒 超高效液相色谱 荧光衍生 检测 贝类 

分 类 号：S944.2[农业科学—水产养殖]