Determination of Brevetoxins in Seawater by Liquid Chromatography-Tandem Mass Spectrometry with Liquid-Liquid Extraction

严忠雍; 曾军杰; 龙举; 方益; 陈思

doi:doi：10.3969/j.issn.1004-4957.2019.12.008

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Determination of Brevetoxins in Seawater by Liquid Chromatography-Tandem Mass Spectrometry with Liquid-Liquid Extraction

- Determination of Brevetoxins in Seawater by Liquid Chromatography-Tandem Mass Spectrometry with Liquid-Liquid Extraction
- Vol. 38, Issue 12, Pages: 1458-1463(2019)
- 作者机构：
  
  1. 浙江省海洋水产研究所
  2. 浙江省海洋渔业资源可持续利用技术研究重点实验室
- 作者简介：
- 基金信息：
- DOI：doi：10.3969/j.issn.1004-4957.2019.12.008
  CLC：
- Published：2019
- 稿件说明：
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严忠雍, 曾军杰, 龙举, 方益, 陈思. Determination of Brevetoxins in Seawater by Liquid Chromatography-Tandem Mass Spectrometry with Liquid-Liquid Extraction[J]. 2019, 38(12): 1458-1463.
DOI：

严忠雍, 曾军杰, 龙举, 方益, 陈思. Determination of Brevetoxins in Seawater by Liquid Chromatography-Tandem Mass Spectrometry with Liquid-Liquid Extraction[J]. 2019, 38(12): 1458-1463. DOI： doi：10.3969/j.issn.1004-4957.2019.12.008.

摘要

建立了基于液液萃取/液相色谱-串联质谱法定量分析海水中3种短裸甲藻毒素(BTX-1、BTX-2、BTX-3)。利用液相色谱-串联质谱的高灵敏度，将海水的分析体积减至20 mL；通过响应面优化确定了海水中短裸甲藻毒素的最佳提取条件：加6 g氯化钠，旋涡时间60 s，用5 mL乙酸乙酯提取2次。3种短裸甲藻毒素的线性范围为1~200 μg/L

其检出限均为0.02 μg/L，定量下限均为0.05 μg/L，平均回收率为95.4%~104%，日内相对标准偏差(RSD)为2.2%~5.3%，日间RSD为3.0%~4.5%。方法降低了样品的分析体积，提高了前处理效率，且时效性和适用性强，实现了污染海水中短裸甲藻毒素的高效率痕量分析。

Abstract

A liquid chromatography-tandem mass spectrometric(LC-MS/MS) method was developed for the detection of three brevetoxins

i.e.BTX-1

BTX-2 and BTX-3 in seawater based on liquid-liquid extraction.The analysis volume of seawater was reduced to 20 mL by using LC-MS/MS.The extraction conditions for three brevetoxins in seawater optimized with response surface were as follows:sodium chloride:6 g

vortex time:60 s

extraction solvent:5 mL ethyl acetate;and extraction times:twice.The linear ranges of three brevetoxins were all 1-200 μg/L

their limits of detection and quantitation were 0.02 μg/L and 0.05 μg/L

respectively.The average recoveries for three brevetoxins ranged from 95.4% to 104%

with intra-day and inter-day relative standard deviations(RSD) of 2.2%-5.3% and 3.0%-4.5%

respectively.With low consumption and high pretreatment efficiency

this method realizes the rapid analysis on trace of brevetoxins in seawater.

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