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热带海洋学报 ›› 2012, Vol. 31 ›› Issue (6): 115-120.doi: 10.11978/j.issn.1009-5470.2012.06.018cstr: 32234.14.j.issn.1009-5470.2012.06.018

• 海洋生物学 • 上一篇    下一篇

超声波提取-固相萃取联用检测河鲀毒素的研究

魏涯, 李来好, 杨贤庆, 岑剑伟, 郝淑贤, 辛少平, 石红, 周婉君   

  1. 中国水产科学研究院南海水产研究所, 广东 广州 510300
  • 收稿日期:2011-04-13 修回日期:2011-06-21 出版日期:2012-12-01 发布日期:2013-02-06
  • 通讯作者: 李来好(1963—), 男, 研究员, 博士生导师, 从事水产品加工与质量安全研究。E-mail: laihaoli@163.com
  • 作者简介:魏涯(1983—), 女, 广东省汕头市人, 硕士, 现从事水产品加工及质量安全方向研究。
  • 基金资助:
    中央级公益性科研院所基本科研业务费专项资金项目(2012TS21); 广东省省级财政专项

Detection of tetrodotoxin in aquatic products using HPLC-UV

WEI Ya, LI Lai-hao, YANG Xian-qing, CEN Jian-wei, HAO Shu-xian, XIN Shao-ping, SHI Hong,ZHOU Wan-jun   

  1. South China Sea Fisheries Research Institute, Chinese Academy of Fishery Sciences, Guangzhou 510300, China
  • Received:2011-04-13 Revised:2011-06-21 Online:2012-12-01 Published:2013-02-06

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被引次数

4 | 2

摘要： 使用热处理、震摇、超声波等手段改善水产品中的河鲀毒素提取率, 利用多种固相萃取柱纯化提取液, 采用高效液相色谱-紫外检测法进行检测, 重点对河鲀毒素的提取和固相萃取纯化进行了研究。试验发现, 结合振荡和加热双重作用的索氏提取法和超声波加热辅助提取法具有较高的提取能力, 其中超声波(35kHz, 强度100%, 60℃)提取10min即可达到最好效果, 耗时短, 效率更高; 比较SCX、PRS、WCX、C18、SAX 5种固相萃取柱对河鲀毒素的吸附作用, SCX、PRS、WCX柱则能够将河鲀毒素完全保留在其上。样品纯化试验结果显示, C18-WCX小柱的组合纯化样品的效果最好, 回收率在75%—82%之间, 相对标准偏差小于15%。研究结果对河鲀毒素的提取、纯化和检测工作具有重要的参考意义。

关键词: 河鲀毒素, 超声波提取, 固相萃取, 高效液相色谱

Abstract: Tetrodotoxin (TTX) accumulated in some aquatic products can be extremely dangerous to human beings. Detecting the content of TTX in aquatic products can help to avoid consuming the toxic products. Due to the complexity of sample composition, TTX detection method has not been developed. The new methods of extracting TTX in puffer fish were studied and presented here. A variety of solid phase extraction column for purification were compared, the high performance liquid chromatography (HPLC) coupled with a UV detector was adopted in the detection. The results showed that both the Soxhlet extraction method and ultrasound treatment method have higher extraction efficiency. Solid-phase extraction (SPE) cartridges were compared in the TTX adsorption experiments, which revealed that the strong cation exchanger (SCX), the propanesulfonic acid SPE cartridge (PRS), and the weak cation exchanger (WCX) had good capacity of retaining TTX. The combination of the octadecyl silane SPE cartridge (C18) and WCX cartridge is even better. The best result can be achieved by extracting 10 min at 35 kHz, 100% intensity, 60℃ ultrasound treatments. The recovery rate is 75%—82%, with the relative standard deviation (RSD) of less than 15%. This newly developed method is efficient and ready to be used in the laboratory.

Key words: tetrodotoxin, extraction, purification, solid-phase extraction (SPE), high performance liquid chromatography (HPLC)

中图分类号: 

  • O657