色谱

色谱

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固相萃取-超过滤-液相色谱/质谱联用法测定织纹螺中的河豚毒素

骆和东,贾玉珠,朱宝平

  

  1. Xiamen Municipal Center for Disease Control and Prevention, Xiamen 361021, China
  • 收稿日期:2007-06-27 修回日期:2007-09-14 出版日期:2007-11-30 发布日期:1984-12-25
  • 通讯作者: 骆和东

Determination of Tetrodotoxin in Nassarius by Solid-Phase Extraction, Ultrafiltration and Liquid
Chromatography-Mass Spectrometry

LUO Hedong, JIA Yuzhu, ZHU Baoping

  

  1. Xiamen Municipal Center for Disease Control and Prevention, Xiamen 361021, China
  • Received:2007-06-27 Revised:2007-09-14 Online:2007-11-30 Published:1984-12-25
  • Contact: LUO Hedong

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摘要：

建立了液相色谱-质谱法测定织纹螺中河豚毒素的分析方法。匀质后的样品用0.03 mol/L乙酸溶液提取,水浴加热10 min,用Sep-Pak C18固相萃取柱净化,再用截留相对分子质量为3000的超滤管过滤。采用Insertsil ODS-3色谱柱分离,以含有30 mmol/L七氟丁酸的甲酸铵溶液(1 mmol/L)-甲醇(体积比为99∶1)为流动相,采用电喷雾离子源,选择离子监测模式检测。以保留时间和河豚毒素的二级质谱特征碎片离子予以定性确证。结果表明,在此分析条件下,可将河豚毒素及其衍生物分离,在0.01～10.0 mg/L范围内线性关系良好(r2＞0.995),检出限(以3倍信噪比为计)为2 μg/L,平均加标回收率为72.5%～80.4%,相对标准偏差为4.48%～8.87%。将该方法用于实际样品检测，在赤潮后所采集的织纹螺样品中检出了河豚毒素。

关键词: 超过滤, 固相萃取, 河豚毒素, 液相色谱-质谱法, 织纹螺

Abstract:

A method for the determination and analysis of tetrodotoxin (TTX) in nassarius using liquid chromatography-mass spectrometry (LC-MS) has been developed.The homogenized sample was extracted with 0.03 mol/L acetic acid by heating in a boiling water-bath for 10 min and then was cleaned up on a Sep-Pak C18 cartridge column and filtered through a Mr3000 cut-off ultrafree microcentrifuge filter. Chromatographic separation was performed on an Insertsil ODS-3 column using 30 mmol/L heptafluorobutyric acid in 1 mmol/L ammonia formate buffer-methanol (99∶1, v/v) as mobile phase at a flow rate of 0.3 mL/min. TTX was identified by retention time in positive mode with selected ion monitoring (SIM).The results showed that TTX and its analogs can be separated with the method. The linear range was 0.01-10.0 mg/L and the correlation coefficients were greater than 0.995 with a detection limit of 2 μg/L (S/N=3). The average recoveries were in the range of 72.5%-80.4% and the relative standard deviations were 4.48%-8.87%. TTX of 0.04-0.50 mg/kg was found in nassarius that was collected from Fujian Province after red tide.

Key words: liquid chromatography-mass spectrometry (LC-MS), nassarius , solid-phase extraction (SPE), tetrodotoxin, ultrafiltration