液相色谱-串联质谱检测鱼类及海鲜类调味品中的雪卡毒素  

Determination of Pacific ciguatoxins in fish&alec samples by liquid chromatography with tandem mass spectrometry

作　　者：周嘉明 姚建华[1,2] 赵华锋 赵峰[2] 李超 周德庆[2] 

机构地区：[1]青岛市华测检测技术有限公司,山东青岛266101 [2]中国水产科学研究院黄海水产研究所,山东青岛266071

出　　处：《中国调味品》2015年第11期105-110,共6页China Condiment

基　　金：国家科技支撑计划资助项目(22012BAK17B13)

摘　　要：建立了液相色谱-串联质谱分析深海鱼及鱼酱中太平洋雪卡毒素（P-CTX-1，P-CTX-2，P-CTX-3）的方法。用甲醇／正己烷（80／20）溶液对太平洋雪卡毒素（P-CTX-1，P-CTX-2，P-CTX-3）进行提取，C18、硅胶固相萃取柱净化后，采用液相色谱分离，以电喷雾离子源正离子选择反应监测模式进行质谱分析。三种太平洋雪卡毒素（P-CTX-1，P-CTX-2，P-CTX-3）在1．0-20μg／L线性良好，相关系数＞0．99。虎鳗肌肉空白样品添加太平洋卡毒素的回收率均在70．1％-93．5％（狀＝6），精密度（RSD）在2．9％-15．3％。鱼肉组织中太平洋雪卡毒素（P-CTX-1，P-CTX-2，P-CTX-3）的检出限均为0．1μg／kg。A liquid chromatography-tandem mass spectrometry （LC-MS/MS ） method for the determination of Pacific ciguatoxins in fish and alec was developed.After being extracted with methanol and hexane （80/20,V/V）,the extraction was cleaned by solid phase extraction of C18column followed by Si column,then determined by a reversed-phase HPLC gradient program coupled with tandem mass spectrometry in multiple reaction monitoring mode.P-CTX-1 ,P-CTX-2 and P-CTX-3 were analyzed in positive ion mode.The calibration curves were good linear between LC peak area of the selected ion-pair and the concentration of P-CTX-1 ,P-CTX-2 and P-CTX-3 with the correlation coefficient over 0 .9 9 . The average recoveries from spiked Strophidon sathete at the three concentrations ranged from 70.1% to 93.5% with relative standard deviation from 2.9% to 15.3%. The limits of detection were 0 .1 0μg/kg for P-CTX-1 ,P-CTX-2 and P-CTX-3 .

关 键 词：太平洋雪卡毒素 鱼肉组织 液相色谱-串联质谱 

分 类 号：TS264.2[轻工技术与工程—发酵工程]