›› 2013, Vol. 25 ›› Issue (5): 0-1113.

• 论文 •    

ASE-SPE-HPLC/MS/MS检测鱼体内的雪卡毒素

周秀锦,周向阳,邵宏宏,颜建波,傅谧妮   

  1. 舟山出入境检验检疫局,浙江 舟山 316000
  • 收稿日期:1900-01-01 修回日期:1900-01-01 出版日期:2013-09-25 发布日期:2013-09-25

Determination of ciguatoxin in coral fish by ASE-SPE-HPLC/MS/MS method

ZHOU Xiu-jin;ZHOU Xiang-yang;SHAO Hong-hong;YAN Jian-bo;FU Mi\|ni   

  • Received:1900-01-01 Revised:1900-01-01 Online:2013-09-25 Published:2013-09-25

摘要: 雪卡毒素中毒是一种全球暴发的海洋食源性疾病,食用含有0.1 μg雪卡毒素的珊瑚鱼即可引起中毒。研究建立了一套快速、高效、高灵敏度的ASE-SPE-HPLC/MS/MS检测方法来保证人类健康,该方法在1.0~50.0 μg·kg-1范围内线性良好,相关系数在0.99以上,检出限为0.03 μg·kg-1,定量下限为0.1 μg·kg-1,基质加标的回收率在95%以上。较之传统方法,该方法有较好的回收率和提取效率。

关键词: 雪卡毒素, 快速溶剂萃取, 固相萃取, 液相色谱-串联质谱

Abstract: Ciguatera fish poisoning (CFP) was a global food-borne illness caused by consumption of sea food containing ciguatoxin (CTX). P-CTX-1 had been suggested to be the most toxic CTX, which caused ciguatera at 01μg in the flesh of carnivorous fish. A sensitive and rapid method for the detection of ciguatoxin in coral fish using ASE-SPE-HPLC/MS/MS was developed in the study. The calibration curve of P-CTX1 showed good linearity in the range of 1.0-50.0 μg·kg-1 with correlation coefficient of 0.99. The validated method had limits of detection (LOD) and quantification (LOQ) of 0.03 μg·kg-1 and 0.1μg·kg-1, respectively, for matrix-based standard solutions, as well as matrix spike recoveries ratio above 95%. Compared with previous methods, this method had better overall recovery and extraction efficiency.

Key words: ciguatoxin, accelerated solvent extraction, solid phase extraction, HPLC-MS/MS